HRID359037
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
A solution of 1-(4-methoxyphenyl)-3-(1-piperazinyl)-1H-indazole hydrochloride (5.0 g, 0.01 mol), nitrourea (4.0 g, 0.04 mol) and dimethylformamide (200 ml) was warmed on a steam bath for 2 hours. The reaction mixture was poured into H2O and the aqueous mixture was extracted with ethyl acetate. The ethyl acetate was dried with MgSO4 and concentrated to 5.3 g of an oil. Crystallization was achieved with toluene affording 3.3 g (65%) of a powder. The powder was recrystallized again from toluene to afford 3.0 g of 4-[1-(4-methoxyphenyl)-1H-indazol-3-yl]-1-piperazine carboxamide, m.p. 155°-157° C.
WORKUP
后处理
- extractionthe aqueous mixture was extracted with ethyl acetate
- dry with materialThe ethyl acetate was dried with MgSO4
- concentrationconcentrated to 5.3 g of an oil
- customCrystallization
- customThe powder was recrystallized again from toluene