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HRID1764948

反应详情

EQUATION

反应方程式

HRID 1764948 的结构方程式

REACTANTS

反应物

2
结构：CCOCC.FB(F)F
HCID8000

Ethane, 1,1'-oxybis-, compd. with trifluoroborane (1:1)

C4H10BF3O

结构：C[C@H](CCC(=O)O)[C@H]1CC=C2C3=C(CC[C@@]21C)[C@@]1(C)CC[C@H](O)C(C)(C)[C@@H]1CC3
HCID69410833

未命名化合物

PRODUCTS

生成物

1
结构：C[C@H](CCC(=O)OC1CCCCC1)[C@H]1CC=C2C3=C(CC[C@@]21C)[C@@]1(C)CC[C@H](O)C(C)(C)[C@@H]1CC3
HCID69411695

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：OC1CCCCC1
溶剂HCID7966

Cyclohexanol

C6H12O

CONDITIONS

反应条件

温度
57.5 °C

PROCEDURE

实验过程

3β-Hydroxy-4,4-dimethyl-5α-chola-8,14-dien-24-oic acid (0.2 g) is suspended in 10 ml of cyclohexanol, 0.1 ml of boron trifluoride diethyl etherate is added and the mixture is stirred at 55-60° C. for 20 hours. After evaporation to dryness under reduced pressure, the remanens is purified by column chromatography and crystallized from methanol to give the title compound (49 mg). Melting point: 130-132° C. 1H-NMR (CDCl3): δ=5.35 (1H, s); 4.75 (1H, m); 3.24 (1H, m). MS: Calculated: 482.8. Found 482.4.

WORKUP

后处理

  1. customAfter evaporation to dryness under reduced pressure
  2. customthe remanens is purified by column chromatography
  3. customcrystallized from methanol