HRID1011240

反应详情

EQUATION

反应方程式

HRID 1011240 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

In a round-bottom flask a suspension of 4-amino-benzoic acid (2 g, 14.58 mmol), C-pyridin-3-yl-methylamine (1.48 mL, 14.58 mmol), hydroxybenzotriazole (HOBt, 2.17 g, 16.04 mmol) and triethylamine (4.06 mL, 29.16 mmol) in dichloromethane (150 mL) is cooled to 0° C. and EDCI*HCl (3.08 g, 16.04 mmol) is added. The reaction mixture is stirred at room temperature for 20 hours. The solvent is removed in vacuo and ice cooled water is added. The precipitate is collected by filtration, washed once with 1 N NaOH, three times with water, two times with petroleum ether and dried in vacuo to give the title compound (2.56 g) as a solid.

WORKUP

后处理

  1. customThe solvent is removed in vacuo and ice
  2. temperaturecooled water
  3. additionis added
  4. filtrationThe precipitate is collected by filtration
  5. washwashed once with 1 N NaOH, three times with water, two times with petroleum ether
  6. customdried in vacuo