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HRID1764949

反应详情

EQUATION

反应方程式

HRID 1764949 的结构方程式

REACTANTS

反应物

4
结构：Cl
HCID313

Hydrochloric Acid

ClH

结构：CN1CCOCC1
HCID7972

4-Methylmorpholine

C5H11NO

结构：CC(C)COC(=O)Cl
HCID62365

Isobutyl chloroformate

C5H9ClO2

结构：C[C@H](CCC(=O)O)[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
HCID69410795

未命名化合物

PRODUCTS

生成物

1
结构：CON(C)C(=O)CC[C@@H](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
HCID87822030

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：ClCCl
溶剂HCID6344

Dichloromethane

CH2Cl2

CONDITIONS

反应条件

温度
-15 °C

PROCEDURE

实验过程

3β-tert-Butyldimethylsilyloxy-4,4-dimethyl-5α-chola-8,14-dien-24-oic acid (5.0 g) is dissolved in 250 ml of dry dichloromethane. After cooling to −15° C., 2.14 ml of N-methylmorpholine and 1.27 ml isobutylchloroformate is added and the mixture is stirred at −15° C. for 20 minutes, whereupon 0.98 g of N,O-dimethylhydroxy/amine, HCl is added and the mixture is stirred overnight and the temperature is slowly elevated to room temperature. After aqueous work-up, 3β-tert-butyldimethylsilyloxy-4,4-dimethyl-5α-chola-8,14-dien-24-oic acid-N-methoxy-N-methyl amide (5.37 g) is obtained. Melting point: 134-135° C. 1H-NMR (CDCl3, 300 MHz): δ=5.35 (1H, s); 3.69 (3H, s); 3.2 (1H, m); 3.18 (3H, s); 0.9 (9H, s); 0.04 (6H, m).

WORKUP

后处理

  1. additionis added
  2. customis slowly elevated to room temperature