HRID736937

反应详情

EQUATION

反应方程式

HRID 736937 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

4.15 g (23.04 mmol) of CDT were added at 0° C. to a suspension of 8.00 g (23.04 mmol) of ethyl 2-amino-3-(4-amino-3-chloro-5-trifluoromethyl-phenyl)-propionate and 16.0 mL (115.00 mmol) of triethylamine in 100 mL of DMF and the mixture was stirred for 1.5 h at 0° C. A solution of 5.64 g (23.00 mmol) of 3-piperidin-4-yl-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one in 200 mL of DMF was added and the mixture was heated to 100° C. for 2 h. The reaction mixture was cooled to RT, diluted with 1.5 L water and stirred for a further 10 min. The precipitate formed was filtered off, washed with water and dried i. vac.

WORKUP

后处理

  1. temperaturethe mixture was heated to 100° C. for 2 h
  2. temperatureThe reaction mixture was cooled to RT
  3. stirringstirred for a further 10 min
  4. customThe precipitate formed
  5. filtrationwas filtered off
  6. washwashed with water
  7. customdried i