تفاعل #1885021
ord-ea1ab50375b34e25b281175bbcaebf43
معادلة التفاعل
2-chloro-5-chloromethylpyridine
2,2-difluoroethan-1-amine
triethylamine
→
N-[(6-chloropyridin-3-yl)methyl]-2,2-difluoroethan-1-amine
المردود 53.9%
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1تركيزAfter concentrating the reaction mixture under reduced pressure, it
- 2غسيلwashed with ethyl acetate
- 3استخلاصextracted repeatedly with ethyl acetate
- 4تركيزConcentrating the organic phase under reduced pressure
الإجراء التجريبي
At 45° C., 41.57 g (256.6 mmol) of 2-chloro-5-chloromethylpyridine, 20.80 g (256.6 mmol) of 2,2-difluoroethan-1-amine and 35.8 ml (256.6 mmol) of triethylamine are stirred in 500 ml of acetonitrile for 21 hours. After concentrating the reaction mixture under reduced pressure, it is taken up with 1 N aqueous hydrochloric acid and washed with ethyl acetate. The aqueous phase is alkalized with 2.5 N aqueous sodium hydroxide solution and extracted repeatedly with ethyl acetate. Concentrating the organic phase under reduced pressure affords 28.6 g (53% of theory) of N-[(6-chloropyridin-3-yl)methyl]-2,2-difluoroethan-1-amine.