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HRID479308

反应详情

EQUATION

反应方程式

HRID 479308 的结构方程式

REACTANTS

反应物

2
结构：Cl
HCID313

Hydrochloric Acid

ClH

结构：C[C@H](CCC(=O)N(C)C)[C@H]1CC=C2C3=C(CC[C@@]21C)[C@@]1(C)CC[C@H](O[Si](C)(C)C(C)(C)C)C(C)(C)[C@@H]1CC3
HCID131724207

未命名化合物

PRODUCTS

生成物

1
结构：C[C@H](CCC(=O)N(C)C)[C@H]1CC=C2C3=C(CC[C@@]21C)[C@@]1(C)CC[C@H](O)C(C)(C)[C@@H]1CC3
HCID69873475

未命名化合物

收率 74.8%

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-dimethyl-5α-chola-8,14-dien-24 oic acid-N,N-dimethyl amide (0.10 g) is dissolved in 5 ml of ethanol, 0.2 ml of 6N hydrogen chloride is added and the mixture is stirred at room temperature the weekend over. The product is precipitated with 10 ml of water, filtered and recrystallized from ethanol/heptan to give the title compound (59 mg). M.p. 192-195° C. 1H-NMR (CDCl3, 400 MHz)): δ=5.36 (1H, s); 3.24 (1H, m); 3.02 (3H, s); 2.94 (3H, s). Molecular weight: Calculated: 427.7. Found (by mass spectroscopy): 427.4.

WORKUP

后处理

  1. customThe product is precipitated with 10 ml of water
  2. filtrationfiltered
  3. customrecrystallized from ethanol/heptan