HRID2209976

反应详情

EQUATION

反应方程式

HRID 2209976 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 6-amino-4-[2-[4-(1H-indol-3-yl)-1-piperidinyl]ethyl]-2(1H)-quinolinone (III-20) (1 g, 2.59 mmol) in dimethylformamide (8 ml) was added triethylamine (0.7 ml, 5 mmol). To the mixture was added dropwise acetyl chloride (0.2 ml, 2.75 mmol) at 0 ° C. and the mixture was stirred at the same temperature for 15 minutes. The reaction mixture was poured into water and the separated solid was filtered off. After washing with water and drying, the solid was recrystallized from a mixture of methanol, tetrahydrofuran and water to give the desired product (III-21) (900 mg) as pale yellow crystals (yield 81.1%, mp 180°-183° C. (methanol/tetrahydrofuran/water).

WORKUP

后处理

  1. filtrationthe separated solid was filtered off
  2. washAfter washing with water
  3. customdrying
  4. customthe solid was recrystallized from a mixture of methanol, tetrahydrofuran and water