huagongshe.com
HRID2187262

反应详情

EQUATION

反应方程式

HRID 2187262 的结构方程式

REACTANTS

反应物

1
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：COC(=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
HCID69411353

未命名化合物

收率 60%

AUXILIARIES

试剂、催化剂与溶剂

2
结构：Cl
溶剂HCID313

Hydrochloric Acid

ClH

结构：CO
溶剂HCID887

Methanol

CH4O

PROCEDURE

实验过程

3β-tert-Butyldimethylsilyloxy-4,4-dimethylchola-5,7-dien-24-oic acid methyl ester (1.0 g) is suspended in a mixture of 25 ml methanol and 3.4 ml of concentrated hydrogen chloride acid and refluxed overnight. After evaporation to dryness under reduced pressure the remanens is triturated with methanol and thereafter recrystallized with methanol/water to give the title compound (0.47 g). Melting point: 156-157° C. 1H-NMR (CDCl3, 400 MHz): δ=5.36 (1H, s); 3.67 (3H, s); 3.23 (1H, m). MS (abbreviation for mass spectroscopy): Calculated: 414.6. Found 414.3.

WORKUP

后处理

  1. temperaturerefluxed overnight
  2. customAfter evaporation to dryness under reduced pressure the remanens
  3. customis triturated with methanol
  4. customrecrystallized with methanol/water