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HRID1087678

反应详情

EQUATION

反应方程式

HRID 1087678 的结构方程式

REACTANTS

反应物

2
结构：O=P(O)(O)O
HCID1004

Phosphoric acid

H3O4P

结构：C[C@]12CCC(=O)C=C1CC[C@H]1[C@@H]3CCC(=O)[C@@]3(C)CC[C@@]12O
HCID10425017

9α-hydroxyandrost-4-en-3,17-dione

C19H26O3

PRODUCTS

生成物

1
结构：C[C@]12CCC(=O)C=C1CC[C@@H]1C2=CC[C@]2(C)C(=O)CC[C@@H]12
HCID239595

9-Dehydroandrostenedione

C19H24O2

AUXILIARIES

试剂、催化剂与溶剂

1
结构：O
溶剂HCID962

Water

H2O

PROCEDURE

实验过程

9α-Hydroxyandrostenedione (280 mg.; 302 mg. of 92.7% purity) is added to phosphoric acid (85%, 5 ml.) and stirred at 35°-48° for 7.5 hours. Water (10 ml.) is then added, the mixture stirred and filtered. The solids are air-dried at 25° for 10 hours to give androsta-4,9(11)-diene-3,17-dione, 254 mg. (90.7% weight yield, 96.2% chemical yield); m.p. 197°-201°. GC (Example 1) shows an androsta-4,9(11)-diene-3,17-dione/androsta-4,8-diene-3,17-dione ratio greater than 99 to 1.

WORKUP

后处理

  1. stirringthe mixture stirred
  2. filtrationfiltered
  3. customThe solids are air-dried at 25° for 10 hours