HRID2394223

反应详情

EQUATION

反应方程式

HRID 2394223 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

In a 500-ml pear-shaped flask, 4-fluorobenzonitrile (10.44 g, 86.26 mmoles), N-methylglycine (8.45 g, 94.89 mmoles) and potassium carbonate (14.28 g, 103.48 mmoles) were placed, followed by addition of 200 ml of dimethylsulfoxide as a solvent. A water cooling pipe was attached to the flask, and the reaction was carried out with heating on an oil bath heated at 100° C. for 9 hours with stirring using a magnetic stirrer. After cooling naturally, the reaction mixture was dissolved in 1 liter of water and subjected to acidolysis with 1/10N HCl, followed by filtration of a precipitate. After washing with water well, the precipitate was washed with hexane/benzene (4/1 in volume ratio). The yield of the product after dried was 14.21 g (74.79 mmoles, 86.7%). The melting point was 64.5° C.

WORKUP

后处理

  1. temperaturewith heating on an oil bath
  2. temperatureAfter cooling naturally
  3. filtrationfollowed by filtration of a precipitate
  4. washAfter washing with water well
  5. washthe precipitate was washed with hexane/benzene (4/1 in volume ratio)
  6. customThe yield of the product after dried