HRID359035

反应详情

EQUATION

反应方程式

HRID 359035 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5.5 g of 3-(1-piperazinyl)-1-[4-(trifluoromethyl)phenyl]-1H-indazole, 4.8 g of nitrourea, and 80 ml of dimethylformamide was heated on a steam bath for 15 minutes. The reaction mixture was then poured into water and the resulting precipitate was collected, washed with water, and dried. The precipitate was purified on a Water's Model 500 Preparative High Pressure Liquid Chromatograph (2×) utilizing two silica gel columns and chloroform/methanol (5%) as the eluent. Concentration of the appropriate fractions yielded a solid which was recrystallized from acetonitrile to afford 2.3 g (37%) of 4-[1-(4-trifluoromethyl)phenyl)-1H-indazol-3-yl]-1-piperazine carboxamide, m.p. 138°-140°.

WORKUP

后处理

  1. temperaturewas heated on a steam bath for 15 minutes
  2. customthe resulting precipitate was collected
  3. washwashed with water
  4. customdried
  5. customThe precipitate was purified on a Water'
  6. customConcentration of the appropriate fractions yielded a solid which
  7. customwas recrystallized from acetonitrile