HRID359037

反应详情

EQUATION

反应方程式

HRID 359037 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. extractionthe aqueous mixture was extracted with ethyl acetate
  2. dry with materialThe ethyl acetate was dried with MgSO4
  3. concentrationconcentrated to 5.3 g of an oil
  4. customCrystallization
  5. customThe powder was recrystallized again from toluene