تفاعل #46777

معادلة التفاعل

1-bromo-3,3,3-trifluoropropan-2-one

hydroxylamine hydrochloride

→

3-bromo-1,1,1-trifluoropropan-2-one oxime

المردود 55.7%

المذيبات

water

chloroform

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe mixture was warmed
2. 2
   درجة الحرارةat reflux
3. 3
   درجة الحرارةthe mixture was cooled
4. 4
   أخرىthe organic phase was separated
5. 5
   استخلاصThe aqueous layer was extracted with three 30 mL portions of methylene chloride
6. 6
   تجفيفThe combined organic layers were dried over sodium sulfate
7. 7
   ترشيحfiltered
8. 8
   تركيزconcentrated in vacuo

الإجراء التجريبي

To a solution of 10.5 mL (102.3 mmol) of 1-bromo-3,3,3-trifluoropropan-2-one in 100 mL of chloroform (passed through a pad of basic Al2O3) was added a solution of 10.4 g (149.7 mmol) of hydroxylamine hydrochloride in 20 mL of water and the mixture was warmed at reflux. After 24 hours, the mixture was cooled and the organic phase was separated. The aqueous layer was extracted with three 30 mL portions of methylene chloride. The combined organic layers were dried over sodium sulfate, filtered, and concentrated in vacuo to afford 11.5 g (55.7%) of 3-bromo-1,1,1-trifluoropropan-2-one oxime as a mixture (3:2) of geometric isomers.

المصدر