HRID65419

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID887

Methanol

CH4O

HCID1118

Sulfuric acid

H2O4S

结构：C[C@]12CC[C@H]3[C@@H]([C@H](Cl)[C@H]4O[C@]45C[C@@H](O[Si](Cc4ccccc4)(Cc4ccccc4)Cc4ccccc4)CC[C@]35C)[C@@H]1[C@@H]1C[C@@H]1C2=O

HCID88687372

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

19 g of 3β-tribenzylsilyloxy-7α-chloro-5,6β-epoxy-15β,16β-methylene-5β-androstan-17-one is dissolved in 50 ml of tetrahydrofuran and 50 ml of methanol and agitated with 15 ml of 8% sulfuric acid for 2 hours at room temperature. The mixture is thereafter diluted with ether, washed with saturated sodium bicarbonate solution and water, dried over sodium sulfate, and concentrated under vacuum. By trituration of the thus-obtained solid with diisopropyl ether, 8.7 g of 7α-chloro-5,6β-epoxy-3β-hydroxy-15β,16β-methylene-5β-androstan-17-one is obtained, mp 172° C.

WORKUP

后处理

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