反応 #684955

反応方程式

Methanesulfonyl chloride

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

Triethylamine

→

title compound

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

溶媒

methylene chloride

反応条件

後処理

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

実験手順

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.

出典