huagongshe.com
HRID918373

反应详情

EQUATION

反应方程式

HRID 918373 的结构方程式

REACTANTS

反应物

2
结构：O=C(OO)c1cccc(Cl)c1
HCID70297

Benzenecarboperoxoic acid, 3-chloro-

C7H5ClO3

结构：C=C(C)CO[C@@H]1C[C@H]2[C@@H]3CCC4=CC(=O)C=C[C@]4(C)[C@@]3(F)[C@@H](O)C[C@]2(C)[C@@]1(O)C(=O)CCl
HCID86733739

未命名化合物

PRODUCTS

生成物

1
结构：CC1(CO[C@@H]2C[C@H]3[C@@H]4CCC5=CC(=O)C=C[C@]5(C)[C@@]4(F)[C@@H](O)C[C@]3(C)[C@@]2(O)C(=O)CCl)CO1
HCID86733741

未命名化合物

收率 14.8%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：ClCCl
溶剂HCID6344

Dichloromethane

CH2Cl2

PROCEDURE

实验过程

A solution of 3.0 g of 21-chloro-9-fluoro-11β,17-dihydroxy-16α-[ (2-methyl-2-propenyl)oxy]pregna-1,4-diene-3,20-dione in 100 ml of dichloromethane is stirred with 1.4 g of m-chloroperbenzoic acid for 210 minutes. The solution is washed with a mixture of 10% potassium carbonate solution and 10% sodium sulfite solution, dried, and evaporated in vacuo to give an oil which solidifies on standing. Recrystallization from acetone-hexane gives 1.94 g as a first crop, and 820 mg as a second crop. Recrystallization of 600 mg of crop 1 from acetone-hexane gives 460 mg of 21-chloro-9-fluoro-11β,17-dihydroxy-16α-[(2-methyloxiranyl)methoxy]pregna-1,4-diene-3,20-dione, melting point 193°-236°C.

WORKUP

后处理

  1. washThe solution is washed with a mixture of 10% potassium carbonate solution and 10% sodium sulfite solution
  2. customdried
  3. customevaporated in vacuo
  4. customto give an oil which
  5. customRecrystallization from acetone-hexane
  6. customgives 1.94 g as a first crop, and 820 mg as a second crop
  7. customRecrystallization of 600 mg of crop 1 from acetone-hexane