huagongshe.com
HRID32297

反应详情

EQUATION

反应方程式

HRID 32297 的结构方程式

REACTANTS

反应物

2
结构：ClCCl
HCID6344

Dichloromethane

CH2Cl2

结构：COC(C)c1cc2c(cc1OCc1ccccc1)CC[C@@H]1[C@@H]2CC[C@]2(C)[C@@H](OC)CC[C@@H]12
HCID68621206

未命名化合物

PRODUCTS

生成物

1
结构：CCc1cc2c(cc1O)CC[C@@H]1[C@@H]2CC[C@]2(C)[C@@H](OC)CC[C@@H]12
HCID68639588

未命名化合物

收率 104.8%

AUXILIARIES

试剂、催化剂与溶剂

3
结构：CC(=O)O
催化剂HCID176

Acetic Acid

C2H4O2

结构：[Pd]
催化剂HCID23938

Palladium

Pd

结构：CCOC(C)=O
溶剂HCID8857

Ethyl acetate

C4H8O2

PROCEDURE

实验过程

290 mg of 2-(1-methoxyethyl)-3-benzyloxy-17β-methoxy-estra-1,3,5(10)-triene was dissolved in 20 ml each of ethyl acetate and dichloromethane and then mixed with 3 drops of acetic acid and 110 mg of palladium on activated carbon (10%). The hydrogenation was carried out under normal pressure over 8 hours. The catalyst was filtered out, and the solution was concentrated by evaporation in a rotary evaporator and co-evaporated several times with toluene. Flash chromatography (toluene/acetone=80:1) yielded 220 mg (98%) of 2-ethyl-3-hydroxy-17β-methoxy-estra-1,3,5(10)-triene as a colorless foam.

WORKUP

后处理

  1. filtrationThe catalyst was filtered out
  2. concentrationthe solution was concentrated by evaporation in a rotary evaporator and co-evaporated several times with toluene