Реакция #67691

ord-46fb6c49246341ae90999280e6b39122

Растворители

Условия реакции

Температура
80°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ЭкстракцияAfter conversion, the product was extracted
  2. 2
    Концентрированиеconcentrated
  3. 3
    Другоеcrystallized in a mixture of xylene/methycyclohexane

Методика

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%)

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08524915B2uspto-grants-2013_09