HRID1778160

反应详情

EQUATION

反应方程式

HRID 1778160 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.2 47 μl (0.61 mmol) of methanesulfonyl chloride is added dropwise with ice-cooling to a suspension of 112.0 mg (0.50 mmol) of 5-bromoisoquinoline 2-oxide in 0.48 ml of pyridine. The reaction mixture is stirred at room temperature for 18 hours. 685 μl of ethanolamine are then added dropwise with ice-cooling, and the mixture is stirred at room temperature for a further 4 hours. The reaction mixture is poured into ice-water and stirred for 30 minutes. The precipitate formed is filtered off with suction, washed with water and dried in vacuo: 5-bromoisoquinolin-1-ylamine as yellow crystals; HPLC/MS: 1.26 min, [M+H] 223/225.

WORKUP

后处理

  1. temperaturecooling
  2. stirringthe mixture is stirred at room temperature for a further 4 hours
  3. stirringstirred for 30 minutes
  4. customThe precipitate formed
  5. filtrationis filtered off with suction
  6. washwashed with water
  7. customdried in vacuo
  8. custom1.26 min, [M+H] 223/225