HRID1252278

反应详情

EQUATION

反应方程式

HRID 1252278 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture consisting of 45 g (0.30 mole) of ethyl 3-ethylaminopropionate, 37.3 g (0.27 mole) of potassium carbonate, 250 ml of toluene and 250 ml of water being stirred in an ice bath was added dropwise 67.7 g (0.45 mole) of ethylmalonyl chloride in 0.5 hour. Stirring was continued for further 3 hours at room temperature and the reaction mixture was subjected to phase separation. The toluene layer obtained was washed with a 5% aqueous HCl solution, a saturated aqueous sodium bicarbonate solution and a saturated aqueous NaCl solution in this order and then dried with anhydrous magnesium sulfate. The resulting solution was subjected to vacuum distillation to remove toluene, whereby 64.3 g of a desired product was obtained with an yield of 83%.

WORKUP

后处理

  1. stirringStirring
  2. customthe reaction mixture was subjected to phase separation
  3. customThe toluene layer obtained
  4. washwas washed with a 5% aqueous HCl solution
  5. dry with materiala saturated aqueous sodium bicarbonate solution and a saturated aqueous NaCl solution in this order and then dried with anhydrous magnesium sulfate
  6. distillationThe resulting solution was subjected to vacuum distillation
  7. customto remove toluene