HRID280107

反应详情

EQUATION

反应方程式

HRID 280107 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

At first, 4 g (0.014 moles) of N-(methylcarbamoyl)-N-(4-trifluoromethylphenyl)-β-alanine was added to a solution consisting of 45 ml of 6N-hydrochloric acid and 15 ml of acetic acid, and the mixture was refluxed with heating for 2 hours. After completion of the reaction, 50 ml of water was added thereto. The deposited crystals were recovered by filtration with suction and recrystallized from ethyl acetate-n-hexane, 3.38 g of the desired compound was obtained as colorless needle crystals having a melting point of 115°-117° C. (yield: 90.1%).

WORKUP

后处理

  1. temperaturethe mixture was refluxed
  2. temperaturewith heating for 2 hours
  3. additionwas added
  4. filtrationThe deposited crystals were recovered by filtration with suction
  5. customrecrystallized from ethyl acetate-n-hexane