HRID1068890
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
Under a nitrogen atmosphere, a suspension of 4.00 g (20.7 mmol) of 5-amino-3-(morpholin-4-yl)-1H-pyrazole-4-carbonitrile in 85 ml of toluene is boiled under reflux for 5 hours with 4.17 ml (97%; 23.6 mmol) of N,N-dimethylformamide diethyl acetal, during which the solid dissolves. Cooling to RT (→crystallization), filtration with suction an d washing with toluene and hexane yield N′-[3-(morpholin-4-yl)-4-cyano-1H-pyrazol-5-yl]-N,N-dimethyl-formamidine; m.p. 182-183° C.; TLC: Rf=0.20 (ethyl acetate).
WORKUP
后处理
- dissolutiondissolves
- filtration(→crystallization), filtration with suction
- washan d washing with toluene and hexane