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HRID918382

反应详情

EQUATION

反应方程式

HRID 918382 的结构方程式

REACTANTS

反应物

2
结构：[O-][I+3]([O-])([O-])O
HCID65185

Metaperiodic acid

HIO4

结构：C[C@]12C=CC(=O)C=C1CC[C@H]1[C@@H]3C[C@@H](OCC4(c5ccccc5)CO4)[C@](O)(C(=O)CCl)[C@@]3(C)C[C@H](O)[C@@]12F
HCID86733746

未命名化合物

PRODUCTS

生成物

1
结构：C[C@]12C=CC(=O)C=C1CC[C@H]1[C@@H]3C[C@@H](OCC(=O)c4ccccc4)[C@](O)(C(=O)CCl)[C@@]3(C)C[C@H](O)[C@@]12F
HCID86733747

未命名化合物

收率 51.3%

AUXILIARIES

试剂、催化剂与溶剂

2
结构：O
溶剂HCID962

Water

H2O

2 次

结构：C1CCOC1
溶剂HCID8028

Tetrahydrofuran

C4H8O

PROCEDURE

实验过程

A solution of 4.8 g of 21-chloro-9-fluoro-11β,17-dihydroxy-16α-[(2-phenyloxiranyl)methoxy]pregna-1,4-diene-3,20-dione in 150 ml of tetrahydrofuran is stirred with a solution of 10 g of periodic acid in 40 ml of water for 4 hours. The resulting slurry is diluted with 1 liter of water and filtered. The solid is dried in vacuo and recrystallized from methanol-chloroform to give 2.4 g of 21-chloro-9-fluoro-11β,17-dihydroxy-16α-(2-oxo-2-phenylethoxy)pregna-1,4-diene-3,20-dione, melting point 266°-268°C, dec.

WORKUP

后处理

  1. filtrationfiltered
  2. customThe solid is dried in vacuo
  3. customrecrystallized from methanol-chloroform