تفاعل #1769436

معادلة التفاعل

ethyl 2-hydroxyisobutyrate

hydrogen fluoride/pyridine

fluorosulfuric acid

→

ethyl 2-fluoroisobutyrate

المردود 52.0%

ظروف التفاعل

المعالجة

1. 1
   أخرىThe resulting mixture was subjected to a reaction at 40° C. for 4 hours
2. 2
   أخرىAfter the completion of the reaction
3. 3
   استخلاصThe resulting mixture was extracted with methylene chloride
4. 4
   تجفيفThe extract was dried over anhydrous sodium sulfate
5. 5
   workup.DISTILLATIONsubjected to vacuum distillation
6. 6
   أخرىto remove methylene chloride
7. 7
   workup.DISTILLATIONThe resulting residue was subjected to distillation

الإجراء التجريبي

Into a 50-ml autoclave having a teflon-made internal cylinder were placed 9 ml of a hydrogen fluoride/pyridine mixture [hydrogen fluoride/pyridne =70/30 (wt/wt), containing about 300 mM of hydrogen fluoride] and 9.15 g (91.5 mM) of fluorosulfuric acid. The autoclave contents were cooled to 0° C. Thereto was added 4.0 g (30.5 mM) of ethyl 2-hydroxyisobutyrate. The resulting mixture was subjected to a reaction at 40° C. for 4 hours. After the completion of the reaction, the reaction mixture was poured into ice water. The resulting mixture was extracted with methylene chloride. The extract was dried over anhydrous sodium sulfate and subjected to vacuum distillation to remove methylene chloride. The resulting residue was subjected to distillation to obtain 2.1 g (yield: 52%) of ethyl 2-fluoroisobutyrate having a boiling point of 124°-126° C.

المصدر