反応 #2254160

反応方程式

2-(3-chloro-2-pyridyl)-5-(trifluoromethyl)pyrazole-3-carbonyl chloride

potassium carbonate

2-amino-3,5-dichloro-N-(diethyl-λ4-sulfanylidene)-benzamide

→

title compound

収率 173.6%

N-[4,6-dichloro-2-[(diethyl-λ4-sulfanylidene)carbamoyl]-phenyl]-2-(3-chloro-2-pyridyl)-5-(trifluoromethyl)pyrazole-3-carboxamide

収率 173.6%

diisopropyl ether

溶媒

acetonitrile

acetonitrile

反応条件

後処理

1. 1
   ろ過The resulting precipitate was collected by filtration
2. 2
   洗浄washed with water and petrol ether

実験手順

A solution of 2-(3-chloro-2-pyridyl)-5-(trifluoromethyl)pyrazole-3-carbonyl chloride (210.7 g, 0.68 mol, 1.10 equiv.) in acetonitrile (500 mL) was added at 22° C. to a suspension of potassium carbonate (103.34 g, 0.74 mol, 1.20 equiv) and 2-amino-3,5-dichloro-N-(diethyl-λ4-sulfanylidene)-benzamide (181.79 g, 0.62 mol, 1.00 equiv) in acetonitrile (2 L). After 2.5 h at this temperature, the reaction mixture was poured into ice-water with stirring. The resulting precipitate was collected by filtration and washed with water and petrol ether. Trituration from diisopropyl ether yielded the crystalline title compound (305 g, 87%).

出典