تفاعل #684955
ord-b181145b20004641a11a34031ada03f5
معادلة التفاعل
الكواشف
المذيبات
ظروف التفاعل
المعالجة
- 1workup.STIRRINGstirred further at room temperature for 2 hours
- 2workup.ADDITIONAfter ice was added
- 3استخلاصthe reaction mixture was extracted with ethyl acetate
- 4غسيلwashed successively with 1 N hydrochloric acid
- 5تجفيفa saturated aqueous sodium hydrogencarbonate solution, and saturated brine, dried over anhydrous magnesium sulfate
- 6ترشيحfiltered through silica gel
- 7تركيزThe filtrate was concentrated under reduced pressure
الإجراء التجريبي
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.