HRID636967

反应详情

EQUATION

反应方程式

HRID 636967 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
170 °C

PROCEDURE

实验过程

Liquid ammonia (220 mL) was added to a solution of 32.8 g of 1-chloro-7-methoxy-isoquinoline in 420 mL of ethanol in a steel vessel. Nitrogen was pressed upon until an initial pressure of 20 atm. was obtained. This reaction mixture was heated for 2 days at 170° C. The solvent was removed in vacuo and the residue dissolved in water. The pH value was adjusted to pH 10 by adding aqueous sodium carbonate solution, followed by extraction with ethyl acetate. The organic extract was washed with brine and dried (Na2SO4). Evaporation of the solvent in vacuo gave pure 7-methoxy-isoquinolin-1-ylamine as a white solid. Yield 24.0 g (81%); m.p. 128-130° C.

WORKUP

后处理

  1. customwas obtained
  2. customThe solvent was removed in vacuo
  3. dissolutionthe residue dissolved in water
  4. additionby adding aqueous sodium carbonate solution
  5. extractionfollowed by extraction with ethyl acetate
  6. extractionThe organic extract
  7. washwas washed with brine
  8. dry with materialdried (Na2SO4)
  9. customEvaporation of the solvent in vacuo