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HRID1764946

反应详情

EQUATION

反应方程式

HRID 1764946 的结构方程式

REACTANTS

反应物

3
结构：c1ccccc1
HCID241

Benzene

C6H6

结构：Cl
HCID313

Hydrochloric Acid

ClH

结构：COC(=O)CC[C@@H](C)[C@H]1CC[C@H]2C3=CC=C4C(C)(C)[C@@H](O[Si](C)(C)C(C)(C)C)CC[C@]4(C)[C@H]3CC[C@]12C
HCID69411642

未命名化合物

PRODUCTS

生成物

1
结构：CCOC(=O)CC[C@@H](C)[C@H]1CC=C2C3=C(CC[C@@]21C)[C@@]1(C)CC[C@H](O)C(C)(C)[C@@H]1CC3
HCID69411949

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CCO
溶剂HCID702

Ethanol

C2H6O

PROCEDURE

实验过程

3β-tert-Butyldimethylsilyloxy-4,4-dimethylchola-5,7-dien-24-oic acid methyl ester (4.0 g) is suspended in a mixture of 60 ml of 96% ethanol, 10.1 ml of benzene and 10.1 ml of concentrated hydrogen chloride acid and refluxed for 3.5 hours. After aqueous work-up and column chromatography followed by crystallization from ethanol the title compound (1.37 g) is isolated. Melting point: 122-124° C. 1H-NMR (CDCl3, 300 MHz): δ=5.35 (1H, s); 4.13 (2H, q); 3.25 (1H, m). 1.25 (3H, t). MS: Calculated: 428.7. Found 428.3.

WORKUP

后处理

  1. temperaturerefluxed for 3.5 hours
  2. customAfter aqueous work-up and column chromatography followed by crystallization from ethanol the title compound (1.37 g)
  3. customis isolated