HRID232902
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe reaction was then refluxed for 6 hours
- customexcess thionyl chloride was removed on a rotary evaporator
- distillationthe residue distilled (boiling point approximately 100° C./1 mbar)
- customwhich crystallized in the receiving flask
- customwas obtained
- customwas 52.2° to 53.1° C