反应 #684955

反应方程式

Methanesulfonyl chloride

N-methyl-N-(2-propynyl)amine

Triethylamine

→

title compound

N-methyl-N-(2-propynyl)methanesulfonamide

溶剂

methylene chloride

反应条件

后处理

1. 1
   workup.STIRRINGstirred further at room temperature for 2 hours
2. 2
   workup.ADDITIONAfter ice was added
3. 3
   萃取the reaction mixture was extracted with ethyl acetate
4. 4
   洗涤washed successively with 1 N hydrochloric acid
5. 5
   干燥a saturated aqueous sodium hydrogencarbonate solution, and saturated brine, dried over anhydrous magnesium sulfate
6. 6
   过滤filtered through silica gel
7. 7
   浓缩The filtrate was concentrated under reduced pressure

实验过程

Triethylamine (6.55 ml) was added to an ice-cooled solution of N-methyl-N-(2-propynyl)amine (2603 mg) in methylene chloride (25 ml). Methanesulfonyl chloride (3.50 ml) was further added dropwise, the reaction mixture was stirred at that temperature for 1 hour, and then stirred further at room temperature for 2 hours. After ice was added, the reaction mixture was extracted with ethyl acetate, washed successively with 1 N hydrochloric acid, a saturated aqueous sodium hydrogencarbonate solution, and saturated brine, dried over anhydrous magnesium sulfate, and then filtered through silica gel. The filtrate was concentrated under reduced pressure to give the title compound (4522 mg). The obtained compound was used in the following reaction without further purification.

来源