HRID621419

反应详情

EQUATION

反应方程式

HRID 621419 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.3 g. (6.3 mMole) 7-amino-4,4-dimethylisoquinoline-1,3-dione was dissolved in 30 ml. pyridine, mixed, while cooling with ice, with 1.5 g. dimethylcarbamoyl chloride and the reaction mixture further stirred for 4 hours at 25° C. Subsequently, the reaction mixture was distilled to dryness, the residue was taken up in methylene chloride, washed with water, dried and the methylene chloride distilled off. The residue was recrystallised from ethanol. Yield 1.1 g. (63.6% of theory); m.p. 256°-258° C.

WORKUP

后处理

  1. temperaturewhile cooling with ice, with 1.5 g
  2. distillationSubsequently, the reaction mixture was distilled to dryness
  3. washwashed with water
  4. customdried
  5. distillationthe methylene chloride distilled off
  6. customThe residue was recrystallised from ethanol