반응 #684955

반응 방정식

Methanesulfonyl chloride

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

Triethylamine

→

title compound

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

용매

methylene chloride

반응 조건

후처리

1. 1
   workup.STIRRINGstirred further at room temperature for 2 hours
2. 2
   workup.ADDITIONAfter ice was added
3. 3
   추출the reaction mixture was extracted with ethyl acetate
4. 4
   세척washed successively with 1 N hydrochloric acid
5. 5
   건조a saturated aqueous sodium hydrogencarbonate solution, and saturated brine, dried over anhydrous magnesium sulfate
6. 6
   여과filtered through silica gel
7. 7
   농축The filtrate was concentrated under reduced pressure

실험 절차

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.

출처