反応 #607873

反応方程式

4-amino-2-chlorophenol

1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxylic acid

EDCI

HOAT

→

title product

収率 72.1%

N-(3-chloro-4-hydroxyphenyl)-1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxamide

収率 72.1%

溶媒

DCM

反応条件

後処理

1. 1
   温度cooled to rt
2. 2
   ろ過filtered
3. 3
   洗浄The filter cake was washed with DCM (20 mL×3)
4. 4
   その他dried at 50° C. in a vacuum oven overnight

実験手順

To a suspension of 4-amino-2-chlorophenol (4.0 g, 28.00 mmol) and 1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxylic acid (7.4 g, 30.11 mmol) in DCM (70 mL) were added EDCI (6.65 g, 30.11 mmol) and HOAT (0.76 g, 5.68 mmol). The mixture was stirred at 45° C. for 20 hours, then cooled to rt and filtered. The filter cake was washed with DCM (20 mL×3), and dried at 50° C. in a vacuum oven overnight to give the title product as a gray solid (7.1 g, 72.1%).

出典