Reaktion #684955

Reaktionsgleichung

Methanesulfonyl chloride

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

Triethylamine

→

title compound

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

Lösungsmittel

methylene chloride

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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.

Quelle