HRID441893

反应详情

EQUATION

反应方程式

HRID 441893 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.1 g. of benzylamine, 7.4 g. of methyl acetate and 1.5 g. of the sodium salt of 4,6-dimethyl-2-hydroxypyridine are dissolved in 30 ml. of dimethyl acetamide and heated at about 78° C. for 4.5 hours. As determined by thin layer chromatography, all but a trace of the benzylamine is consumed. 200 ml. of water and 0.9 ml. of concentrated hydrochloric acid are added to the reaction solution, and the solution is extracted three times with 100 ml. of ethyl acetate. The organic layer is washed with 100 ml. of water, and, after drying with sodium sulfate, concentrated and crystallized. Recrystallization from 300 ml. of ether-petroleum benzin (1:1), 2.5 g. of needle-like crystals of N-benzyl acetamide are obtained (yield: 84 percent). m.p. 60.5° - 62° C.

WORKUP

后处理

  1. customall but a trace of the benzylamine is consumed
  2. additionof concentrated hydrochloric acid are added to the reaction solution
  3. extractionthe solution is extracted three times with 100 ml
  4. washThe organic layer is washed with 100 ml
  5. dry with materialof water, and, after drying with sodium sulfate
  6. concentrationconcentrated
  7. customcrystallized
  8. customRecrystallization from 300 ml