反応 #67691

反応方程式

9-Dichloromethylene-1,2,3,4-tetrahydro-1,4-methano-naphthalen-5-ylamine

triethylamine

3-Difluoromethyl-1-methyl-1H-pyrazole-4-carbonyl chloride

→

pure product

収率 83.4%

3-difluoromethyl-1-methyl-1H-pyrazole-4-carboxylic acid (9-dichloromethylene-1,2,3,4-tetrahydro-1,4-methano-naphthalen-5-yl)-amide

収率 83.4%

溶媒

xylene

反応条件

後処理

1. 1
   抽出After conversion, the product was extracted
2. 2
   濃縮concentrated
3. 3
   その他crystallized in a mixture of xylene/methycyclohexane

実験手順

9-Dichloromethylene-1,2,3,4-tetrahydro-1,4-methano-naphthalen-5-ylamine (166 g, 35% xylene solution, 0.25 mol), triethylamine (28 g, 0.275 mol) and xylene (13 g) were charged in a reactor and the mixture was heated to 80° C. 3-Difluoromethyl-1-methyl-1H-pyrazole-4-carbonyl chloride (182 g, 26% xylene solution, 0.25 mol) was added over 2 hours. After conversion, the product was extracted, concentrated and crystallized in a mixture of xylene/methycyclohexane. 83 g of pure product were isolated. (Purity: 97%, Yield: 82%)

出典