HRID868169

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID9845

Trifluoroacetic anhydride

C4F6O3

结构：C=C1C[C@@H]2C(=CC[C@@]3(C)[C@H]2C[C@H](C)[C@]3(O)C(C)=O)[C@@]2(C)CCC(=O)C=C12

HCID13477372

未命名化合物

PRODUCTS

生成物

结构：C=C1C[C@@H]2C(=CC[C@@]3(C)[C@H]2C[C@H](C)[C@]3(OC(C)=O)C(C)=O)[C@@]2(C)CCC(=O)C=C12

HCID13477374

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID176

Acetic Acid

C2H4O2

PROCEDURE

实验过程

A solution of 3.3 g of 17α-hydroxy-16β-methyl-6-methylene-4,9(11)-pregnadiene-3,20-dione in 40 ml of glacial acetic acid is cooled to 0° C. and stirred, after adding 15 ml of trifluoroacetic acid anhydride dropwise, for one hour at room temperature. After precipitation into ice water-sodium chloride, the mixture is filtered off and worked up as usual. The crude product is purified on 450 g of silica gel with a hexane-ethyl acetate gradient (0-50% ethyl acetate), thus obtaining 2.3 g of 17α-acetoxy-16β-methyl-6-methylene-4,9(11)-pregnadiene-3,20-dione, mp 197°-198° C.

WORKUP

后处理

customAfter precipitation into ice water-sodium chloride
filtrationthe mixture is filtered off
customThe crude product is purified on 450 g of silica gel with a hexane-ethyl acetate gradient (0-50% ethyl acetate)