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HRID1277611

反应详情

EQUATION

反应方程式

HRID 1277611 的结构方程式

REACTANTS

反应物

3
结构：CCOC(C)=O
HCID8857

Ethyl acetate

C4H8O2

结构：O=C1NC(=O)C(Br)(Br)N1
HCID54068228

未命名化合物

结构：CC(=O)OCC(=O)[C@@]1(OC(C)=O)[C@@H](C)C[C@H]2[C@@H]3C[C@H](F)C4=CC(=O)C=C[C@]4(C)C3=CC[C@@]21C
HCID70369648

未命名化合物

PRODUCTS

生成物

1
结构：CC(=O)OCC(=O)[C@@]1(OC(C)=O)[C@@H](C)C[C@H]2[C@@H]3C[C@H](F)C4=CC(=O)C=C[C@]4(C)[C@@]3(Br)[C@@H](O)C[C@@]21C
HCID22815480

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：O
溶剂HCID962

Water

H2O

结构：C1COCCO1
溶剂HCID31275

1,4-Dioxane

C4H8O2

PROCEDURE

实验过程

Ten (10) g of 6α-fluoro-16β-methyl-17α,21-diacetoxypregna-1,4,9(11)-triene-3,20-dione in 110 ml of dioxane (A.R.) plus 2.2 mls of a solution of 4.4 ml 70% HClO4 in 200 mls of water, is treated with 4 g of dibromohydantoin in the dark at R.T. for a period of one hour or when TLC using 50% ethyl acetate/50% hexane shows the reaction to be complete. The reaction mixture is precipitated in 2 l of water, stirred for 10 minutes and the crystalline precipitate collected by filtration, washed with water, and air dried to give 11.4 g of 6α-fluoro-9α-bromo-11β-hydroxy-16β-methyl-17α,21-diacetoxypregna-1,4-diene-3,20-dione.

WORKUP

后处理

  1. customthe reaction
  2. customThe reaction mixture is precipitated in 2 l of water
  3. filtrationthe crystalline precipitate collected by filtration
  4. washwashed with water, and air
  5. customdried