反応 #1265371

反応方程式

pivaloylacetonitrile

p-tolylhydrazine hydrochloride

Heptane

→

5-Amino-3-t-butyl-1-p-tolylpyrazole hydrochloride

溶媒

methanol

反応条件

後処理

1. 1
   その他methanol was removed by distillation
2. 2
   その他The product was crystallized from the solution
3. 3
   ろ過collected by filtration
4. 4
   その他dried in vacuum oven to constant weight

実験手順

A solution of pivaloylacetonitrile (750 g, 6.0 mol) and p-tolylhydrazine hydrochloride (660 g, 4.2 mol) in methanol (2.8 L) was refluxed for 3 h. Heptane was added, and methanol was removed by distillation. The product was crystallized from the solution, collected by filtration and dried in vacuum oven to constant weight. Yield: 1.05 kg, 94%. 1H NMR □CDCl3) 7.50 (d, 2H), 7.30 (d, 2H), 5.60 (s, 1H), 2.45 (s, 3H), 1.40 (s, 9H). MS (CI) m/z 229 (M++H).

出典