HRID2296343

反应详情

EQUATION

反应方程式

HRID 2296343 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1 G. of the 3-cyano-2-oxotridecanoic acid ethyl ester is dissolved in 5 ml of methanesulfonic acid and the mixture allowed to stand overnight at room temperature. The reaction mixture is worked up by first pouring into ethanol-water (20 ml ethanol--5 ml water). After standing for several hours, the ethanol is removed by evaporation. The aqueous acidic residue is diluted further with water and then extracted with chloroform. The chloroform solution is then washed well with water, dried and evaporated to give the desired 3-hydroxy-4-(n-decyl)-3-pyrroline-2,5-dione. Recrystallization from hexane or cyclohexane provides pure 3-hydroxy-4-(n-decyl)-3-pyrroline-2,5-dione, mp 109°-111° C.

WORKUP

后处理

  1. waitAfter standing for several hours
  2. customthe ethanol is removed by evaporation
  3. additionThe aqueous acidic residue is diluted further with water
  4. extractionextracted with chloroform
  5. washThe chloroform solution is then washed well with water
  6. customdried
  7. customevaporated