huagongshe.com
HRID1973728

反应详情

EQUATION

反应方程式

HRID 1973728 的结构方程式

REACTANTS

反应物

3
结构：O
HCID962

Water

H2O

结构：C=CC(=O)[C@H]1CC[C@H]2[C@@H]3CC[C@H]4C[C@H](O)CC[C@]4(C)[C@H]3C(=O)C[C@]12C
HCID86734286

未命名化合物

结构：OC(=S)CN1CCOCC1
HCID178526202

未命名化合物

PRODUCTS

生成物

1
结构：C[C@]12CC[C@@H](O)C[C@@H]1CC[C@H]1[C@@H]3CC[C@H](C(=O)CCSC(=O)CN4CCOCC4)[C@@]3(C)CC(=O)[C@@H]12
HCID86734297

未命名化合物

收率 66.8%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CC(C)=O
溶剂HCID180

Acetone

C3H6O

PROCEDURE

实验过程

3α-Hydroxy-21-methylene-5α-pregnane-11,20-dione (500 mg) was dissolved in acetone (20 ml) and the solution treated with morpholinothioacetic acid (300mg), at reflux for 3 hours. The mixture was poured into water and the emulsion extracted with either. The extracts were washed with water, dried over anhydrous sodium sulphate and evaporated to a foam (540 mg) which was purified by preparative t.l.c. in ethyl acetate/petrol (1:1). The main band gave title compound (490mg.) as a white foam. [α]D + 48° (c = 1.03).

WORKUP

后处理

  1. temperatureat reflux for 3 hours
  2. extractionthe emulsion extracted with either
  3. washThe extracts were washed with water
  4. dry with materialdried over anhydrous sodium sulphate
  5. customevaporated to a foam (540 mg) which
  6. customwas purified by preparative t.l.c