HRID2059936

反应详情

EQUATION

反应方程式

HRID 2059936 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1,1-Dimethylethyl 6-cyano-5-methyl-3,4-dihydro-2(1H)-isoquinolinecarboxylate (Preparation 16; 404 mg; 1.48 mmol) was stirred overnight at 80° C. with hydroxylamine hydrochloride (619 mg; 8.90 mmol) and sodium bicarbonate (748 mg; 8.9 mmol) in ethanol (10 ml). Further sodium bicarbonate (400 mg) and hydroxylamine hydrochloride (300 mg) were added, and heating continued for ca. 8 h. The mixture was cooled to room temperature, and the resulting solid removed, washed with ethanol, and dried under high vacuum to give the title compound as a white solid (431 mg).

WORKUP

后处理

  1. temperatureheating
  2. customthe resulting solid removed
  3. washwashed with ethanol
  4. customdried under high vacuum