HRID1590532

反应详情

EQUATION

反应方程式

HRID 1590532 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.67 g of methacryloyl chloride in 5 ml of chloroform were added dropwise to 5 g of 2-[N-(p-nitrophenyl)-N-methylamino]-ethanol and 2.02 g of pyridine in 40 ml of chloroform while cooling. Thereafter, the resulting reaction solution was first stirred at room temperature and then refluxed for 3.5 hours. It was cooled to room temperature and then 40 ml of water were added to it, after which the chloroform phase was separated off and the aqueous phase was extracted with three times 20 ml of chloroform. After the combined chloroform phases had been dried with Na2SO4 and the chloroform evaporated off, the resulting product was washed with hexane and dried under reduced pressure. 2.6 g of 2-[N-(p-nitrophenyl)-N-methylamino]-ethyl methacrylate were obtained, the IR spectrum of the product in the form of a KBr pellet having bands at 2,950, 2,900, 1,720, 1,600, 1,510, 1,490, 1,320, 1,310, 1,160, 1,110 and 825 cm-1.

WORKUP

后处理

  1. temperaturewhile cooling
  2. customThereafter, the resulting reaction solution
  3. temperaturerefluxed for 3.5 hours
  4. temperatureIt was cooled to room temperature
  5. customafter which the chloroform phase was separated off
  6. extractionthe aqueous phase was extracted with three times 20 ml of chloroform
  7. dry with materialAfter the combined chloroform phases had been dried with Na2SO4
  8. customthe chloroform evaporated off
  9. washthe resulting product was washed with hexane
  10. customdried under reduced pressure