HRID1462939

反应详情

EQUATION

反应方程式

HRID 1462939 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.54 g of (R,S)-1-(p-methoxybenzoyl)-2-oxo-3-pyrrolidinylchloroacetate are heated at 100° C. in 50 ml of pyridine for 10 minutes under nitrogen with 0.42 g of thiourea and 7 ml of ethanol. The solvent is removed by evaporation and the residue is partitioned between ethyl acetate and water. The organic phase is washed several times with water and the aqueous phases are extracted with ethyl acetate. The combined ethyl acetate phases are evaporated, the residue is boiled at reflux in diisopropyl ether and then the solution is decanted off from insoluble constituents. The clear, colourless diisopropyl ether phase is stirred in an ice-bath and then left to stand in an ice box overnight. The product which crystallises out is filtered off and there is obtained (R,S)-1-(p-methoxybenzoyl)-3-hydroxy-2-pyrrolidinone of melting point 125°-126° C.

WORKUP

后处理

  1. customThe solvent is removed by evaporation
  2. customthe residue is partitioned between ethyl acetate and water
  3. washThe organic phase is washed several times with water
  4. extractionthe aqueous phases are extracted with ethyl acetate
  5. customThe combined ethyl acetate phases are evaporated
  6. temperatureat reflux in diisopropyl ether
  7. customthe solution is decanted off from insoluble constituents
  8. waitleft
  9. customThe product which crystallises out
  10. filtrationis filtered off