HRID512809

反应详情

EQUATION

反应方程式

HRID 512809 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
2.5 °C

PROCEDURE

实验过程

A mixture of residue containing methyl 2-(benzyloxy)propanoate compound of formula-12 obtained in step-a) and water (500 ml) was cooled to 0-5° C. A solution of sodium hydroxide (51.5 g) in water (375 ml) was added to reaction mixture at 0-5° C. and stirred the reaction mixture for 1 hour at the same temperature. Temperature of the reaction mixture was raised to 25-30° C. and stirred for 4 hours at this temperature. After completion of the reaction, washed the reaction mixture with dichloromethane. Both dichloromethane and aqueous layers were separated and pH of aqueous layer was adjusted to 2.5 using 50% hydrochloric acid solution. Extracted the aqueous layer with dichloromethane. Distilled off the solvent from dichloromethane layer under reduced pressure to get the title compound as a residue. The obtained residue can be taken into next step without isolation.

WORKUP

后处理

  1. additionA mixture of residue
  2. temperatureTemperature of the reaction mixture was raised to 25-30° C.
  3. stirringstirred for 4 hours at this temperature
  4. customAfter completion of the reaction
  5. washwashed the reaction mixture with dichloromethane
  6. customBoth dichloromethane and aqueous layers were separated
  7. extractionExtracted the aqueous layer with dichloromethane
  8. distillationDistilled off the solvent from dichloromethane layer under reduced pressure