反应 #2320145

反应方程式

2,3-Dichlorobenzamide

dimethylformamide dimethylacetal

→

title compound

2,3-dichloro-N-[(dimethylamino)methylene]benzamide

反应条件

后处理

1. 1
   温度at reflux for 1.5 hours
2. 2
   浓缩concentrated under reduced pressure
3. 3
   其他the residue was partitioned between diethyl ether and water
4. 4
   洗涤The organic phase was washed with water (2×), saturated sodium chloride
5. 5
   干燥dried with sodium sulfate
6. 6
   过滤filtered
7. 7
   浓缩the filtrate was concentrated under reduced pressure
8. 8
   其他The residue was purified by flash chromatography
9. 9
   洗涤eluting with ethyl acetate

实验过程

2,3-Dichlorobenzamide (4.96 g, 26.1 mmol) and dimethylformamide dimethylacetal (10 mL) were heated at reflux for 1.5 hours, allowed to cool to room temperature, concentrated under reduced pressure, and the residue was partitioned between diethyl ether and water. The organic phase was washed with water (2×), saturated sodium chloride, dried with sodium sulfate, filtered, and the filtrate was concentrated under reduced pressure. The residue was purified by flash chromatography eluting with ethyl acetate to provide the title compound. MS (DCI/NH3) m/z 245 (M+H)+.

来源