HRID25476

反应详情

EQUATION

反应方程式

HRID 25476 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
37.5 °C

PROCEDURE

实验过程

85 g of methyl 4-(2-(phthalimido)ethoxy)acetoacetate was agitated with 31.7 ml of 2-chlorobenzaldehyde and 37 ml of 2-propanol at 20-25° C. The solution of 1.1 ml of piperidine in 14 ml of 2-propanol was added dropwise during 1.5 hour. The mixture was than agitated for 2 hours at the same temperature and for 2 hours at 35-40° C. The mixture was acidified with 1.5 ml of acetic acid, 140 ml of 2-propanol was added and the solution was cooled to 0-5° C. The isopropanolic layer was separated and the organic layer was again washed with 53 ml of 2-propanol. The organic layer, containing the desired product, was evaporated to dryness in order to remove the residual solvent.

WORKUP

后处理

  1. additionwas added
  2. temperaturethe solution was cooled to 0-5° C
  3. customThe isopropanolic layer was separated
  4. washthe organic layer was again washed with 53 ml of 2-propanol
  5. additionThe organic layer, containing the desired product
  6. customwas evaporated to dryness in order
  7. customto remove the residual solvent