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HRID328212

反应详情

EQUATION

反应方程式

HRID 328212 的结构方程式

REACTANTS

反应物

3
结构：O
HCID962

Water

H2O

结构：CC[C@]12CC[C@@H]3c4ccc(OC)cc4CC[C@H]3[C@@H]1C[C@H]1O[C@H]12
HCID86734624

未命名化合物

结构：[Li]C(C)(C)C
HCID178418306

未命名化合物

PRODUCTS

生成物

1
结构：CC[C@]12CC[C@@H]3c4ccc(OC)cc4CC[C@H]3[C@@H]1C=C[C@H]2O
HCID86734623

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：CCOCC
溶剂HCID3283

Diethyl Ether

C4H10O

2 次

结构：CCCCC
溶剂HCID8003

Pentane

C5H12

PROCEDURE

实验过程

At 0° C. and under argon, 4 ml. of a 2-molar tert.-butyllithium solution in pentane is added to 450 mg. of 16α,17α-epoxy-3-methoxy-18-methyl-1,3,5(10)-estratriene in 12 ml. of ether. After 1 hour, the solution is diluted with ether, gently mixed with water, washed neutral, and dried over sodium sulfate. After purifying the crude product by preparative layer chromatography (system: hexane/ethyl acetate = 7 : 3), 140 mg. of 3-methoxy-18-methyl-1,3,5(10),15-estratetraen-17α-ol is obtained as an oily product. [α]D 20 = -105°.

WORKUP

后处理

  1. customAt 0° C.
  2. washwashed neutral
  3. dry with materialdried over sodium sulfate
  4. customAfter purifying the crude product by preparative layer chromatography (system: hexane/ethyl acetate = 7 : 3), 140 mg