HRID1155599

反应详情

EQUATION

反应方程式

HRID 1155599 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

225 ml of 37 weight percent aqueous formaldehyde solution are added dropwise with stirring to a solution of 316 g of diethyl 2-oxo-3-phenylsuccinate sodium salt and 560 ml of water. During the addition, the mixture is maintained at a temperature below 25° C. The mixture is stirred for one hour at room temperature and then 152 g of anhydrous K2CO3 are added in portions over a ten minute period, while the temperature is maintained below 25° C. The resultant mixture is vigorously stirred for 1.5 hours at room temperature under a nitrogen atmosphere. The reaction mixture is diluted with 1500 ml of water and extracted with one 2.5 l. portion of ether followed by two 1.25 l portions of ether. The ether is removed and a product comprising an oil of ethyl atropate is obtained.

WORKUP

后处理

  1. additionDuring the addition
  2. temperaturethe mixture is maintained at a temperature below 25° C
  3. temperatureis maintained below 25° C
  4. extractionextracted with one 2.5 l
  5. customThe ether is removed
  6. customis obtained