تفاعل #168720

معادلة التفاعل

N-[1-(3-Bromo-phenyl)-2,2-difluoro-1-hydroxymethyl-ethyl]-2-chloro-acetamide

potassium tert-butoxide

water

→

title compound

5-(3-Bromo-phenyl)-5-difluoromethyl-morpholin-3-one

المذيبات

tert-butanol

ظروف التفاعل

المعالجة

1. 1
   أخرىthe reaction was evaporated
2. 2
   أخرىThe phases were separated
3. 3
   استخلاصthe aqueous phase was extracted twice with ethyl acetate
4. 4
   غسيلThe organic phases were washed with water and brine
5. 5
   تجفيفdried over Na2SO4
6. 6
   تركيزconcentrated under reduced pressure

الإجراء التجريبي

N-[1-(3-Bromo-phenyl)-2,2-difluoro-1-hydroxymethyl-ethyl]-2-chloro-acetamide (8.10 g, 23.65 mmol) and potassium tert-butoxide (5.31 g, 47.3 mmol) were heated to 95° C. in 118 ml tert-butanol for 30 minutes. After completion water was added and the reaction was evaporated. The residue was put between ethyl acetate and water. The phases were separated and the aqueous phase was extracted twice with ethyl acetate. The organic phases were washed with water and brine, dried over Na2SO4 and concentrated under reduced pressure to yield the title compound as off-white solid. 1H-NMR (360 MHz, DMSO-d6): 9.13 (s, 1H, NH), 7.78 (s, 1H), 7.59 (m, 2H), 7.42 (t, 1H), 6.48 (t, 1H, CHF2), 4.28 (d, 1H), 4.10 (m, 2H), 3.92 (m, 1H); MS: 306 [(M+H)+].

المصدر