HRID2166247

反应详情

EQUATION

反应方程式

HRID 2166247 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into a 500 ml reaction flask equipped with a stirrer, a thermometer, a condenser and a dropping funnel, 48.3 g (0.2 mol) of 2-anilino-4-methyl-6-acetonyl-pyrimidine and 200 ml of toluene were charged and dissolved. To this solution, 61.4 g (0.4 mol) of phosphorus oxychloride was dropwise added from the dropping funnel. The mixture was reacted at a temperature of from 88° to 90° C. for further 6 hours. The reaction mixture was cooled and put into a water/toluene solution and subjected to liquid separation. The toluene layer was washed with an aqueous sodium carbonate solution and then with water. The toluene layer was concentrated to obtain 49 g of 2-anilino-4-methyl-6-(2-chloropropen-1-yl)pyrimidine having a melting point of from 63° to 66° C. The yield was 94.4%.

WORKUP

后处理

  1. customInto a 500 ml reaction flask
  2. customequipped with a stirrer
  3. dissolutiondissolved
  4. customThe mixture was reacted at a temperature of from 88° to 90° C. for further 6 hours
  5. temperatureThe reaction mixture was cooled
  6. customsubjected to liquid separation
  7. washThe toluene layer was washed with an aqueous sodium carbonate solution
  8. concentrationThe toluene layer was concentrated