反应 #65154

反应方程式

3-Chloropropylsulfonyl chloride

3-chloropropylsulfonyl chloride

methylamine hydrochloride

potassium carbonate

→

N-methyl-3-chloropropylsulfonamide

收率 74.0%

溶剂

ethyl acetate

反应条件

后处理

1. 1
   干燥dried over anhydrous sodium sulfate
2. 2
   过滤The mixture was filtered through a small amount of silica gel
3. 3
   浓缩the filtrate was concentrated in vacuo

实验过程

3-Chloropropylsulfonyl chloride 1 (6.8 g,94.9 mmol), methylamine hydrochloride (13.5 g,200 mmol), and potassium carbonate (27.6 g,200 mmol) were added in turn to ethyl acetate (500 ml). After the addition of N-benzyltrimethylammonium chloride (about 200 mg), the resultant mixture was stirred for 2 hours at room temperature and dried over anhydrous sodium sulfate. The mixture was filtered through a small amount of silica gel and the filtrate was concentrated in vacuo to give 12 g (74%) of crude N-methyl-3-chloropropylsulfonamide (intermediate 3b) as a pale yellow oil.

来源