反应详情

温度

20 °C

To a solution of 2-chlorobenzoylacetonitrile (400 g, 2.23 mol) in ethanol (9 L) was added hydrazine hydrate (221 g, 4.42 mol) over 15 minutes while maintaining internal reaction temperature at 15 to 25° C. The mixture was then heated at 75° C. for 20 hr. After cooling, the reaction was concentrated, in vacuo, to give a brown oil. The residue was dissolved in ethyl acetate (4 L), washed with half saturated brine (4 L), and then dried (Na2SO4) to a give a crude, dark orange solution of 5-(2-chlorophenyl)-2H-pyrazol-3-ylamine that was carried directly into the next reaciton: +ESI MS (M+1) 194.0.

1. temperatureThe mixture was then heated at 75° C. for 20 hr
2. temperatureAfter cooling
3. concentrationthe reaction was concentrated, in vacuo
4. customto give a brown oil
5. washwashed with half saturated brine (4 L)
6. dry with materialdried (Na2SO4) to