HRID979209
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- additionA suspension of 7.3 g
- distillationSubsequently, excess ester is distilled off in a vacuum
- customthe residue obtained
- customis separated on silica gel (elution agent: dichloromethane/ammonia-saturated methanol 20:1 v/v)
- customm.p. 333°-337° C. (recrystallised from water/methanol 10:1 v/v)