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HRID1577860

反应详情

EQUATION

反应方程式

HRID 1577860 的结构方程式

REACTANTS

反应物

2
反应SMILES：[O-][Cl+3]([O-])([O-])O
HCID24247

Perchloric acid

HClO4

反应SMILES：CC(=O)OCC(=O)[C@H]1[C@H](C)C[C@H]2[C@@H]3C[C@H](Cl)C4=CC(=O)C=C[C@]4(C)[C@H]3[C@@H](O)C[C@@]21C
HCID70518265

未命名化合物

PRODUCTS

产物

1
反应SMILES：C[C@@H]1C[C@H]2[C@@H]3C[C@H](Cl)C4=CC(=O)C=C[C@]4(C)[C@H]3[C@@H](O)C[C@]2(C)[C@H]1C(=O)CO
HCID70516972

未命名化合物

收率 75.3%

AUXILIARIES

试剂、催化剂与溶剂

1
反应SMILES：CO
溶剂HCID887

Methanol

CH4O

PROCEDURE

实验过程

1.5 g of 21-acetoxy-6α-chloro-11β-hydroxy-16α-methyl-1,4-pregnadiene-3,20-dione is dissolved in 42 ml of methanol; 1.3 ml of 70% perchloric acid is added thereto and the mixture allowed to stand at room temperature for 20 minutes. The reaction mixture is stirred into ice water, the thus-obtained precipitate is filtered off, washed with water, and dried in the open air. After recrystallization from acetone-diisopropyl ether, 1.02 g of 6α-chloro-11β,21-dihydroxy-16α-methyl-1,4-pregnadiene-3,20-dione is obtained, m.p. 128° C. [α]D25 =+55° (chloroform).

WORKUP

后处理

  1. filtrationthe thus-obtained precipitate is filtered off
  2. washwashed with water
  3. customdried in the open air
  4. customAfter recrystallization from acetone-diisopropyl ether