HRID1837271

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID887

Methanol

CH4O

HCID1049

Pyridine

C5H5N

HCID6101

4-Methylbenzenesulfonic acid

C7H8O3S

HCID7918

Acetic anhydride

C4H6O3

结构：C[C@]12C[C@@H](O)[C@H]3[C@@H](CCC4=CC(=O)CC[C@@H]43)[C@@H]1CCC2=O

HCID10902298

11alpha-Hydroxy-estr-4-ene-3,17-dione

C18H24O3

PRODUCTS

生成物

结构：CC(=O)OC1=CC2=CC[C@@H]3[C@H]([C@H](OC(C)=O)C[C@]4(C)C(=O)CC[C@@H]34)[C@H]2CC1

HCID69918053

未命名化合物

CONDITIONS

反应条件

温度: -30 °C

PROCEDURE

实验过程

10 g of p-toluenesulfonic acid is added to 100 g of 11α-hydroxy-estr-4-ene-3,17-dione in 1 liter of acetic anhydride at room temperature. After 5 hours, the solution is stirred into pyridine-containing ice/water, the precipitated product is suctioned off and washed neutral with water. The water-moistened crude product that is obtained is mixed with 200 ml of methanol, stirred for 30 minutes at −30° C., the crystallizate is suctioned off, washed with cold methanol and dried in a vacuum at 50° C. 115 g of 3,11α-diacetoxy-estra-3,5-dien-17-one is obtained.

WORKUP

后处理

washwashed neutral with water
customThe water-moistened crude product that is obtained
washwashed with cold methanol
customdried in a vacuum at 50° C