HRID1088935

反应详情

EQUATION

反应方程式

HRID 1088935 的结构方程式

PROCEDURE

实验过程

A suspension of 7.3 g. (0.038 mol) 5,6-diamino-3,3-dimethylindolin-2-one in 11.6 g. (0.077 mol) methyl 4-pyridylacetate is heated, while stirring, under an atmosphere of nitrogen for about 16 hours to 180° C. Subsequently, excess ester is distilled off in a vacuum and the residue obtained is separated on silica gel (elution agent: dichloromethane/ammonia-saturated methanol 20:1 v/v). Yield: 1.8 g. (16% of theory); m.p. 333°-337° C. (recrystallised from water/methanol 10:1 v/v).

WORKUP

后处理

  1. additionA suspension of 7.3 g
  2. distillationSubsequently, excess ester is distilled off in a vacuum
  3. customthe residue obtained
  4. customis separated on silica gel (elution agent: dichloromethane/ammonia-saturated methanol 20:1 v/v)
  5. customm.p. 333°-337° C. (recrystallised from water/methanol 10:1 v/v)