Reaktion #67691

Reaktionsgleichung

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

Ausbeute 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

Ausbeute 83.4%

Lösungsmittel

xylene

Reaktionsbedingungen

Aufarbeitung

1. 1
   ExtraktionAfter conversion, the product was extracted
2. 2
   Einengenconcentrated
3. 3
   Sonstigecrystallized in a mixture of xylene/methycyclohexane

Vorschrift

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%)

Quelle