HRID1649468

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID887

Methanol

CH4O

HCID1118

Sulfuric acid

H2O4S

结构：CC(C)(C)[Si](C)(C)O[C@H]1CC[C@]2(C)[C@H]3CC[C@]4(C)C(=O)[C@H]5C[C@H]5[C@H]4[C@@H]3[C@H](Cl)[C@H]3O[C@]32C1

HCID13075964

未命名化合物

PRODUCTS

生成物

HCID7914

Isopropyl ether

C6H14O

结构：C[C@]12CC[C@H]3[C@@H]([C@H](Cl)[C@H]4O[C@]45C[C@@H](O)CC[C@]35C)[C@@H]1[C@@H]1C[C@@H]1C2=O

HCID13075966

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID3283

Diethyl Ether

C4H10O

溶剂HCID8028

Tetrahydrofuran

C4H8O

PROCEDURE

实验过程

142 g of 3β-(tert.-butyldimethylsilyloxy)-7α-chloro-5,6β-epoxy-15β,16β-methylene-5β-androstan-17-one is dissolved in 400 ml of tetrahydrofuran and 400 ml of methanol and stirred with 1,000 ml of 8% strength sulfuric acid for 1.5 hours at room temperature. The mixture is then diluted with ether, washed with saturated sodium bicarbonate solution and water, dried over sodium sulfate, and concentrated under vacuum. By trituration of the resultant solid with diisopropyl ether, 108 g of 7α-chloro-5,6β-epoxy-3β-hydroxy-15β,16β-methylene-5β-androstan-17-one is obtained, mp 173° C.

WORKUP

后处理

washwashed with saturated sodium bicarbonate solution and water
dry with materialdried over sodium sulfate
concentrationconcentrated under vacuum