HRID1578119

反应详情

EQUATION

反应方程式

HRID 1578119 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

17 g (0.11 mol) of phenylacetylchloride were added dropwise in 30 minutes and at room temperature, to a solution of N-(1-carbomethoxy-ethyl)-2,6-dimethyl-aniline(21.2 g at a purity of 95%, 0.1 mol) in toluene (150 ml) and dimethylformamide (1 ml.). The reaction mixture was stirred 1 hour at room temperature and 3 hours at reflux temperature, then it was cooled down to room temperature and washed with an aqueous solution of NaHCO3 at 5% and successively with water. The organic phase was separated and anhydrified with anhydrous Na2SO4. The solvent was evaporated and the rough product obtained was recrystallized from ligroin (75°-120° C.), so obtaining 26 g. of the desired product (white solid, m.p. 78°-80° C.).

WORKUP

后处理

  1. temperatureat reflux temperature
  2. temperatureit was cooled down to room temperature
  3. washwashed with an aqueous solution of NaHCO3 at 5% and successively with water
  4. customThe organic phase was separated
  5. customThe solvent was evaporated
  6. customthe rough product obtained
  7. customwas recrystallized from ligroin (75°-120° C.)
  8. customso obtaining 26 g