asymmetric total synthesis and biosynthetic implications

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Literature 08/20/2021 Asymmetric Total Synthesis and Biosynthetic Implications of Perovskones, Hydrangenone, and Hydrangenone B Yu Wang Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375 R O Me Me H O O Me Me H Me Me R R n, n=1 or 2 R

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Page 1: Asymmetric Total Synthesis and Biosynthetic Implications

Literature 08/20/2021

Asymmetric Total Synthesis and Biosynthetic Implications of Perovskones, Hydrangenone, and Hydrangenone B

Yu Wang

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

ROMe

MeH

O

O

MeMe

H

Me

Me

R

R

n, n=1 or 2

R

Page 2: Asymmetric Total Synthesis and Biosynthetic Implications

Introduction

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

• Triterpenoids isolated from Salvia plants• Featuring a complex heptacyclic framework

• Hydrangenone - analogues to the family of

triterpenoids with unprecedented 6/7/6/5/5 skeleton

OMe

MeH

O

O

MeMeH

Me

Me

Perovskone

Me

MeH

O

O

MeMeH

Me

Me

OHO Me

OH

Hydrangenone

Me

Page 3: Asymmetric Total Synthesis and Biosynthetic Implications

Introduction

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

• Triterpenoids isolated from Salvia plants• Featuring a complex heptacyclic framework

• Hydrangenone - analogues to the family of

triterpenoids with unprecedented 6/7/6/5/5 skeleton

OMe

MeH

O

O

MeMeH

Me

Me

Perovskone

Me

MeH

O

O

MeMeH

Me

Me

OHO Me

OH

Hydrangenone

Me

Page 4: Asymmetric Total Synthesis and Biosynthetic Implications

Proposed Biosynthesis

Parve. A, Iqbal Choudhary. M, Akhter. F, Norwalk. M, Mohammad. F. V, Hasan. N. M, Zamir. T, Ahmad. V, J. Org. Chem. 1992, 57, 16, 4339-4340

Perovskone

Me

MeH

O

OMe

MeOH

Precursor of icetexone

MeMe

Me

O

H

PO

OH

OP OH

O OH

Geranyl pyrophosphate

MeOMe

MeH

O

O

MeMe

H

Me

Me

Perovskone

Page 5: Asymmetric Total Synthesis and Biosynthetic Implications

Proposed Biosynthesis

Tabefam. M, Farimani. M, Danton. O, Ramseyer. J, Ebrahimi. S, Neuburger. M, Kaiser. M, Salehi. P, Potterat. O, Hamburger. M, J. Nat. Prod. 2018, 81, 2682-2691

Hydrangenone B

Me

OOP

OH

OH

1-deoxy-D-xylulose 5-P

Dehydration Me

OOP

OH

+PO

Me

Me

DMAPP

POO Me

Me

OMeH

B

Me

MeH

O

OMe

MeOH

Me

MeH

OH

Me

O

O

Me

Me

Me

HO

O

3+2 Cycloaddtion

Me

MeH

OH

Me

O

O

Me

Me

Me

HO

Ene-reaction

Me

MeH

O

O

MeMe

H

OO

O

Me

Me

Me

O

Me

MeH

O

O

MeMe

H

OOHH

O

Me

Me

MeReduction

Hydrangenone B

Page 6: Asymmetric Total Synthesis and Biosynthetic Implications

Synthetic Overview

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

MeOMe

MeH

O

O

MeMe

H

Me

Me

Perovskone

MeOMe

MeH

O

O

MeMe

H

Me

Me

OPerovskone C

MeOMe

MeH

O

O

MeMe

H

Me

Me

O

OH

Perovskone D

MeOMe

MeH

O

O

MeMe

H

Me

Me

O

OH

Perovskone F

Me

MeH

O

O

MeMe

H

Me

Me

OHO Me

OH

Hydrangenone

Me

MeH

O

O

MeMe

H

OOHH

O

Me

Me

Me

Hydrangenone B

Me

MeH

Perovskatone D

O

OMe

MeOH

OH

Page 7: Asymmetric Total Synthesis and Biosynthetic Implications

Synthetic Plan

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

Me

MeH

Perovskatone D

O

OMe

MeOH

OH

Me Me

trans-α-ocimene

Asymmetric Photoenolization Diels-Alder Reaction

Me MeCHO

OBnOMe

Me

Me

OMeOMe

Me

OHC

MeOMe

MeH

O

O

MeMe

H

Me

Me

Perovskone

cycloaddition, cyclization

Me

MeH

O

O

MeMe

H

Me

Me

OHO Me

OH

Hydrangenone

Me

MeH

O

O

MeMe

H

OOHH

O

Me

Me

Me

Hydrangenone B

oxidativecleavage

recyclization

MeOMe

MeH

O

O

MeMe

H

Me

Me

olefinmigration

oxidativecleavage

recyclizationPerovskone C, D, F

selective oxidation

Page 8: Asymmetric Total Synthesis and Biosynthetic Implications

Synthetic Plan

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

Me

MeH

Perovskatone D

O

OMe

MeOH

OH

Me Me

trans-α-ocimene

Asymmetric Photoenolization Diels-Alder Reaction

Me MeCHO

OBnOMe

Me

Me

OMeOMe

Me

OHC

MeOMe

MeH

O

O

MeMe

H

Me

Me

Perovskone

cycloaddition, cyclization

Me

MeH

O

O

MeMe

H

Me

Me

OHO Me

OH

Hydrangenone

Me

MeH

O

O

MeMe

H

OOHH

O

Me

Me

Me

Hydrangenone B

oxidativecleavage

recyclization

MeOMe

MeH

O

O

MeMe

H

Me

Me

olefinmigration

oxidativecleavage

recyclizationPerovskone C, D, F

selective oxidation

Page 9: Asymmetric Total Synthesis and Biosynthetic Implications

Synthetic Plan

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

Me

MeH

Perovskatone D

O

OMe

MeOH

OH

Me Me

trans-α-ocimene

Asymmetric Photoenolization Diels-Alder Reaction

Me MeCHO

OBnOMe

Me

Me

OMeOMe

Me

OHC

MeOMe

MeH

O

O

MeMe

H

Me

Me

Perovskone

cycloaddition, cyclization

Me

MeH

O

O

MeMe

H

Me

Me

OHO Me

OH

Hydrangenone

Me

MeH

O

O

MeMe

H

OOHH

O

Me

Me

Me

Hydrangenone B

oxidativecleavage

recyclization

MeOMe

MeH

O

O

MeMe

H

Me

Me

olefinmigration

oxidativecleavage

recyclizationPerovskone C, D, F

selective oxidation

Page 10: Asymmetric Total Synthesis and Biosynthetic Implications

Synthetic Plan

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

Me

MeH

Perovskatone D

O

OMe

MeOH

OH

Me Me

trans-α-ocimene

Asymmetric Photoenolization Diels-Alder Reaction

Me MeCHO

OBnOMe

Me

Me

OMeOMe

Me

OHC

MeOMe

MeH

O

O

MeMe

H

Me

Me

Perovskone

cycloaddition, cyclization

Me

MeH

O

O

MeMe

H

Me

Me

OHO Me

OH

Hydrangenone

Me

MeH

O

O

MeMe

H

OOHH

O

Me

Me

Me

Hydrangenone B

oxidativecleavage

recyclization

MeOMe

MeH

O

O

MeMe

H

Me

Me

olefinmigration

oxidativecleavage

recyclizationPerovskone C, D, F

selective oxidation

Page 11: Asymmetric Total Synthesis and Biosynthetic Implications

Synthesis of Perovskones and HydrangenonesForward Synthesis-Key Step

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

Me MeCHO

OBnOMe

Me

Me

OMeOMe

Me

OHC+

3 steps from commercial material

4 steps from commercial material

OBn

O

H

O

MeO OMe

Me

Me

TiiPrO

Ti

OMeOiPr

O iPrOiPrO OOiPr*L1

Me

Me

hv (λ=366nm)2.4 equiv Ti(OiPr)4

0.15 equiv TADDOL type ligand L1DCM, 1.5 h

94% yield d.r.=20:1

endo-selectivity

OBnOH

OMe

OMe

Me

MeOMe

MeMe

OHC

94.5:5.5 er97.7:2.3 er after recrystallization

MeO

MeOOHOH

F3C

CF3 F3C

CF3

CF3

F3C

F3C

CF3

L1

X-ray analysis

Page 12: Asymmetric Total Synthesis and Biosynthetic Implications

Synthesis of Perovskones and HydrangenonesForward Synthesis

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

OBnOH

OMe

OMe

Me

MeOMe

MeMe

OHCIBX, DMSO

80 °C, 10h

OBnO

OMe

OMe

Me

MeOMe

MeMe

OHC

73% yield

1) PdCl2, H2, EtOH/DCM(1:1)

r.t., 18h2) Li(t-BuO)3AlH, THF

-78°C to 0 °C

OHO

OMe

OMe

Me

MeOMe

MeMe

HO

92% yield over 2 steps

I2, PPh3, quinoline

toluene(dry), 60 °C, 3.5h91% yield

OHO

OMe

OMe

Me

MeOMe

MeMe

I

AIBN, Bu3SnHtoluene(dry and degassed)

90 °C, 8h

OH

OMe

OMe

Me

MeOMe

MeMe

O

Me

MeH

MeO

OMeMe

MeOMe

OH

O

Me

MeH

MeO

OMeMe

MeOMe

O

OH

+

68% yield total

Page 13: Asymmetric Total Synthesis and Biosynthetic Implications

Synthesis of Perovskones and HydrangenonesForward Synthesis

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

OBnOH

OMe

OMe

Me

MeOMe

MeMe

OHCIBX, DMSO

80 °C, 10h

OBnO

OMe

OMe

Me

MeOMe

MeMe

OHC

73% yield

1) PdCl2, H2, EtOH/DCM(1:1)

r.t., 18h2) Li(t-BuO)3AlH, THF

-78°C to 0 °C

OHO

OMe

OMe

Me

MeOMe

MeMe

HO

92% yield over 2 steps

I2, PPh3, quinoline

toluene(dry), 60 °C, 3.5h91% yield

OHO

OMe

OMe

Me

MeOMe

MeMe

I

AIBN, Bu3SnHtoluene(dry and degassed)

90 °C, 8h

OH

OMe

OMe

Me

MeOMe

MeMe

O

Me

MeH

MeO

OMeMe

MeOMe

OH

O

Me

MeH

MeO

OMeMe

MeOMe

O

OH

+

68% yield total

Page 14: Asymmetric Total Synthesis and Biosynthetic Implications

Synthesis of Perovskones and HydrangenonesForward Synthesis

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

OBnOH

OMe

OMe

Me

MeOMe

MeMe

OHCIBX, DMSO

80 °C, 10h

OBnO

OMe

OMe

Me

MeOMe

MeMe

OHC

73% yield

1) PdCl2, H2, EtOH/DCM(1:1)

r.t., 18h2) Li(t-BuO)3AlH, THF

-78°C to 0 °C

OHO

OMe

OMe

Me

MeOMe

MeMe

HO

92% yield over 2 steps

I2, PPh3, quinoline

toluene(dry), 60 °C, 3.5h91% yield

OHO

OMe

OMe

Me

MeOMe

MeMe

I

AIBN, Bu3SnHtoluene(dry and degassed)

90 °C, 8h

OH

OMe

OMe

Me

MeOMe

MeMe

O

Me

MeH

MeO

OMeMe

MeOMe

OH

O

Me

MeH

MeO

OMeMe

MeOMe

O

OH

+

68% yield total

Page 15: Asymmetric Total Synthesis and Biosynthetic Implications

Synthesis of Perovskones and HydrangenonesForward Synthesis

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

OBnOH

OMe

OMe

Me

MeOMe

MeMe

OHCIBX, DMSO

80 °C, 10h

OBnO

OMe

OMe

Me

MeOMe

MeMe

OHC

73% yield

1) PdCl2, H2, EtOH/DCM(1:1)

r.t., 18h2) Li(t-BuO)3AlH, THF

-78°C to 0 °C

OHO

OMe

OMe

Me

MeOMe

MeMe

HO

92% yield over 2 steps

I2, PPh3, quinoline

toluene(dry), 60 °C, 3.5h91% yield

OHO

OMe

OMe

Me

MeOMe

MeMe

I

AIBN, Bu3SnHtoluene(dry and degassed)

90 °C, 8h

OH

OMe

OMe

Me

MeOMe

MeMe

O

Me

MeH

MeO

OMeMe

MeOMe

OH

O

Me

MeH

MeO

OMeMe

MeOMe

O

OH

+

68% yield total

Page 16: Asymmetric Total Synthesis and Biosynthetic Implications

Synthesis of Perovskones and HydrangenonesForward Synthesis

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

Me

MeH

MeO

OMeMe

MeOMe

OH

O

Me

MeH

MeO

OMeMe

MeOMe

O

OH

+1) Li, NH3/THF (1:1), -100 °C, 1h

2) DDQ, toulene, r.t., 3hMe

MeH

MeO

OMeMe

MeOMe

OH

47% yield over 2 stepsdr=4.7:1 (trans:cis)

AgO

dioxane/6N HNO3, 10 °C69% yield total

Me

MeH

O

OMe

MeOMe

OH Me

MeH

O

OMe

MeOH

OH+

Product Ratio: 6.7:1

Perovskatone DMethyl-Perovskatone D

Page 17: Asymmetric Total Synthesis and Biosynthetic Implications

Synthesis of Perovskones and HydrangenonesForward Synthesis

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

Me

MeH

MeO

OMeMe

MeOMe

OH

O

Me

MeH

MeO

OMeMe

MeOMe

O

OH

+1) Li, NH3/THF (1:1), -100 °C, 1h

2) DDQ, toulene, r.t., 3hMe

MeH

MeO

OMeMe

MeOMe

OH

47% yield over 2 stepsdr=4.7:1 (trans:cis)

AgO

dioxane/6N HNO3, 10 °C69% yield total

Me

MeH

O

OMe

MeOMe

OH Me

MeH

O

OMe

MeOH

OH+

Product Ratio: 6.7:1

Perovskatone DMethyl-Perovskatone D

Page 18: Asymmetric Total Synthesis and Biosynthetic Implications

Synthesis of Perovskones and HydrangenonesForward Synthesis

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

Me

MeH

O

OMe

MeOR

OH

R=H, Perovskatone DR=Me, Methyl-Perovskatone D

+MeMe

1 step from commercial material

Eu(fod)3, toluene

60°C

Me

Me

O

OR

iPr

Me

Me

H

OHODiels-Alder

Reaction

endo-selectivity

Me

MeH

OH

Me

Me

O

O

Me

MeOR

hemiacetalization

Me

MeH

O

Me

Me

O

HO

Me

MeOH LiCl

DMSOonepot

OCF3CF2CF2

OMe

MeMe

Eu

3

Page 19: Asymmetric Total Synthesis and Biosynthetic Implications

Synthesis of Perovskones and HydrangenonesCascade Cyclization- Perovskone and Derivative

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

Me

MeH

O

Me

Me

O

HO

Me

MeOHBi(OTf)3, DCM

20°C, 4hMe

MeH

O

Me

Me Me

O

Me

MeOH

OMe

MeH

O

O

MeMe

H

Me

Me

Perovskone

OMe

MeH

O

O

MeMe

H

Me

Me

Perovskone derivative

+

63% yield over 2 steps

Product ratio: 1.5:1Me

Me

Page 20: Asymmetric Total Synthesis and Biosynthetic Implications

Synthesis of Perovskones and HydrangenonesCascade Cyclization- Perovskone and Derivative

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

Me

MeH

O

Me

Me

O

HO

Me

MeOHBi(OTf)3, DCM

20°C, 4hMe

MeH

O

Me

Me Me

O

Me

MeOH

OMe

MeH

O

O

MeMe

H

Me

Me

Perovskone

OMe

MeH

O

O

MeMe

H

Me

Me

Perovskone derivative

+

63% yield over 2 steps

Product ratio: 1.5:1Me

Me

Page 21: Asymmetric Total Synthesis and Biosynthetic Implications

Synthesis of Perovskones and HydrangenonesCascade Cyclization- Perovskone and Derivative

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

Me

MeH

O

Me

Me

O

HO

Me

MeOHBi(OTf)3, DCM

20°C, 4hMe

MeH

O

Me

Me Me

O

Me

MeOH

OMe

MeH

O

O

MeMe

H

Me

Me

Perovskone

OMe

MeH

O

O

MeMe

H

Me

Me

Perovskone derivative

+

63% yield over 2 steps

Product ratio: 1.5:1Me

Me

Page 22: Asymmetric Total Synthesis and Biosynthetic Implications

Synthesis of Perovskones and HydrangenonesForward Synthesis

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

Me

MeH

O

Me

Me

O

HO

Me

MeOHCu(OTf)2, DCM,

80°C, 4.5-5 hO

Me

MeH

O

O

MeMe

H

Me

Me

Me

OMe

MeH

O

O

MeMe

H

Me

Me

Perovskone derivative

Me

43% yield over 2 steps from perovskatone56% yield over 2 steps from methyl-perovskatone

cation intermediate

OMe

MeH

O

O

MeMe

H

Me

Me

Perovskone derivative

Me

O3, Me2S, DCM

-78°C, 2 min OOMe

MeH

O

O

MeMe

H

Me

Me

Me O

50% yield

Pyrrolidine, AcOH

toluene, 90 °C, 1.5 h Me

MeH

O

O

MeMe

H

Me

Me

OHO Me

OH

Hydrangenone

91% yield

Page 23: Asymmetric Total Synthesis and Biosynthetic Implications

Synthesis of Perovskones and HydrangenonesForward Synthesis

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

Me

MeH

O

Me

Me

O

HO

Me

MeOHCu(OTf)2, DCM,

80°C, 4.5-5 hO

Me

MeH

O

O

MeMe

H

Me

Me

Me

OMe

MeH

O

O

MeMe

H

Me

Me

Perovskone derivative

Me

43% yield over 2 steps from perovskatone56% yield over 2 steps from methyl-perovskatone

cation intermediate

OMe

MeH

O

O

MeMe

H

Me

Me

Perovskone derivative

Me

O3, Me2S, DCM

-78°C, 2 min OOMe

MeH

O

O

MeMe

H

Me

Me

Me O

50% yield

Pyrrolidine, AcOH

toluene, 90 °C, 1.5 h Me

MeH

O

O

MeMe

H

Me

Me

OHO Me

OH

Hydrangenone

91% yield

Page 24: Asymmetric Total Synthesis and Biosynthetic Implications

Synthesis of Perovskones and HydrangenonesForward Synthesis

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

Me

MeH

O

Me

Me

O

HO

Me

MeOHCu(OTf)2, DCM,

80°C, 4.5-5 hO

Me

MeH

O

O

MeMe

H

Me

Me

Me

OMe

MeH

O

O

MeMe

H

Me

Me

Perovskone derivative

Me

43% yield over 2 steps from perovskatone56% yield over 2 steps from methyl-perovskatone

cation intermediate

OMe

MeH

O

O

MeMe

H

Me

Me

Perovskone derivative

Me

O3, Me2S, DCM

-78°C, 2 min OOMe

MeH

O

O

MeMe

H

Me

Me

Me O

50% yield

Pyrrolidine, AcOH

toluene, 90 °C, 1.5 h Me

MeH

O

O

MeMe

H

Me

Me

OHO Me

OH

Hydrangenone

91% yield

Page 25: Asymmetric Total Synthesis and Biosynthetic Implications

Synthesis of Perovskones and HydrangenonesForward Synthesis

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

OMe

MeH

O

O

MeMe

H

Me

Me

Perovskone

Me

O3, Me2S, DCM

-78°C, 1.5 min

42% yield

OMe

MeH

O

O

MeMe

H

Me

Me

OMeOHC

Me

MeH

O

O

MeMe

H

OOHH

O

Me

Me

Me

Hydrangenone B

Page 26: Asymmetric Total Synthesis and Biosynthetic Implications

Synthesis of Perovskones and HydrangenonesForward Synthesis

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

OMe

MeH

O

O

MeMe

H

Me

Me

Perovskone derivative

Me

Na2CrO4, NaOAc, 60°Ctoluene, AcOH/Ac2O

MeOMe

MeH

O

O

MeMe

H

Me

Me

OPerovskone C

1)NaBH4, CeCl3, MeOH, -78°C,20min

MeOMe

MeH

O

O

MeMe

H

Me

Me

O

OH

Perovskone F

17% yield

1) SeO2, dioxane 100°C, 1.5h

2) DMP, DCM16°C, 30min

19% yield over 2 steps

MeOMe

MeH

O

O

MeMe

H

Me

Me

O

OH

Perovskone D82% yield, d.r.=1.8:12) m-CPBA, NaHCO3DCM, 0°C, 1h67% yield

Page 27: Asymmetric Total Synthesis and Biosynthetic Implications

Synthesis of Perovskones and HydrangenonesForward Synthesis

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

OMe

MeH

O

O

MeMe

H

Me

Me

Perovskone derivative

Me

Na2CrO4, NaOAc, 60°Ctoluene, AcOH/Ac2O

MeOMe

MeH

O

O

MeMe

H

Me

Me

OPerovskone C

1)NaBH4, CeCl3, MeOH, -78°C,20min

MeOMe

MeH

O

O

MeMe

H

Me

Me

O

OH

Perovskone F

17% yield

1) SeO2, dioxane 100°C, 1.5h

2) DMP, DCM16°C, 30min

19% yield over 2 steps

MeOMe

MeH

O

O

MeMe

H

Me

Me

O

OH

Perovskone D82% yield, d.r.=1.8:12) m-CPBA, NaHCO3DCM, 0°C, 1h67% yield

Page 28: Asymmetric Total Synthesis and Biosynthetic Implications

Synthesis of Perovskones and HydrangenonesForward Synthesis

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

OMe

MeH

O

O

MeMe

H

Me

Me

Perovskone derivative

Me

Na2CrO4, NaOAc, 60°Ctoluene, AcOH/Ac2O

MeOMe

MeH

O

O

MeMe

H

Me

Me

OPerovskone C

1)NaBH4, CeCl3, MeOH, -78°C,20min

MeOMe

MeH

O

O

MeMe

H

Me

Me

O

OH

Perovskone F

17% yield

1) SeO2, dioxane 100°C, 1.5h

2) DMP, DCM16°C, 30min

19% yield over 2 steps

MeOMe

MeH

O

O

MeMe

H

Me

Me

O

OH

Perovskone D82% yield, d.r.=1.8:12) m-CPBA, NaHCO3DCM, 0°C, 1h67% yield

Page 29: Asymmetric Total Synthesis and Biosynthetic Implications

Synthesis of Perovskones and Hydrangenones

Baochao Yang, Guoen Wen, Quan Zhang, Min Hou, Haibing He, Shuanhu Gao, J. Am. Chem. Soc. 2021, 143, 6370-6375

MeOMe

MeH

O

O

MeMe

H

Me

Me

Perovskone

MeOMe

MeH

O

O

MeMe

H

Me

Me

OPerovskone C

MeOMe

MeH

O

O

MeMe

H

Me

Me

O

OH

Perovskone D

MeOMe

MeH

O

O

MeMe

H

Me

Me

O

OH

Perovskone F

Me

MeH

O

O

MeMe

H

Me

Me

OHO Me

OH

Hydrangenone

Me

MeH

O

O

MeMe

H

OOHH

O

Me

Me

Me

Hydrangenone B

- 19-24 steps from commercial avaliable materials

-asymmetric PEDA

- stereospecific Diels-Alder reaction followed by cascade cyclization

produced perovskone

-selective oxidations produced other members in the natural product

family