HRID325969
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
To 10 g of ice water was added 1.84 g of cyanuric chloride dissolved in 50 ml of acetone. To this solution kept at an internal temperature of 0° to 5° C. under stirring were added 1.68 g of sodium bicarbonate and 1.40 g of glycine ethylester hydrochloride and the mixture was stirred at said temperature for 30 minutes. The reaction product was extracted with ethyl acetate and dried with sodium sulfate. Then, ethyl acetate was distilled out and separated crystal was recrystallized from cyclohexane to obtain 1.3 g of 4,6-dichloro-2-ethoxycarbonylmethylamino-S-triazine which had a melting point of 89° to 90.5° C.
WORKUP
后处理
- customkept at an internal temperature of 0° to 5° C.
- stirringthe mixture was stirred
- customfor 30 minutes
- extractionThe reaction product was extracted with ethyl acetate
- dry with materialdried with sodium sulfate
- distillationThen, ethyl acetate was distilled out
- customseparated crystal
- customwas recrystallized from cyclohexane