HRID2111903

反应详情

EQUATION

反应方程式

HRID 2111903 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Portions of 1,1′-carbonyldiimidazole (2.06 g, 12.7 mmol) are added to a stirred mixture of isoquinoline-1-carboxylic acid (2.00 g, 11.6 mmol) in dichloromethane (25 ml). N,O-dimethylhydroxylamine hydrochloride (1.24 g, 12.7 mmol) is added and the mixture is stirred at ambient temperature overnight. The reaction mixture is diluted with dichloromethane and then washed with saturated aqueous sodium bicarbonate followed by saturated aqueous sodium chloride. The organic solution is dried with sodium sulfate, filtered, and concentrated to give 2.5 g of N-methyl N-methoxy isoquinoline-1-carboxamide, which is used in the next step without further purification: mass spectrum (ion spray): m/z=217.0 (M+1).

WORKUP

后处理

  1. washwashed with saturated aqueous sodium bicarbonate
  2. dry with materialThe organic solution is dried with sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated