HRID232902

反应详情

EQUATION

反应方程式

HRID 232902 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

12 drops of dimethylformamide was added to a solution of 3.0 g (18.9 mmol) of 2-chloropyrimidine-4-carboxylic acid in 60 ml of thionyl chloride. The reaction was then refluxed for 6 hours. After cooling to room temperature, excess thionyl chloride was removed on a rotary evaporator and the residue distilled (boiling point approximately 100° C./1 mbar). 2.95 g of product, corresponding to a yield of 88 percent relative to the 2-chloropyrimidine-4-carboxylic acid used, which crystallized in the receiving flask, was obtained. The melting point of the product was 52.2° to 53.1° C. Other data for the product was:

WORKUP

后处理

  1. temperatureThe reaction was then refluxed for 6 hours
  2. customexcess thionyl chloride was removed on a rotary evaporator
  3. distillationthe residue distilled (boiling point approximately 100° C./1 mbar)
  4. customwhich crystallized in the receiving flask
  5. customwas obtained
  6. customwas 52.2° to 53.1° C