تفاعل #45287

معادلة التفاعل

1-(1,4-dioxa-8-aza-spiro[4.5]dec-8-yl)-2,2,2-trifluoroethanone

→

8-(2,2,2-trifluoroethyl)-1,4-dioxa-8-aza-spiro[4.5]decane

المردود 100.8%

المذيبات

THF

borane methyl sulfide

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter refluxing the reaction mixture for 12 h
2. 2
   درجة الحرارةthe reaction was cooled
3. 3
   أخرىquenched with MeOH
4. 4
   أخرىAfter removal of THF
5. 5
   استخلاصthe residue was extracted with ethyl acetate
6. 6
   غسيلwashed with brine
7. 7
   تجفيفdried with MgSO4
8. 8
   تركيزconcentrated

الإجراء التجريبي

In the solution of 1-(1,4-dioxa-8-aza-spiro[4.5]dec-8-yl)-2,2,2-trifluoroethanone (20 g, 83.7 mmol) in THF, borane-methyl sulfide complex (83.7 mL, 2M solution in THF) was added at 0° C. After refluxing the reaction mixture for 12 h, the reaction was cooled and quenched with MeOH. After removal of THF, the residue was extracted with ethyl acetate and washed with brine, dried with MgSO4 and concentrated to give 8-(2,2,2-trifluoroethyl)-1,4-dioxa-8-aza-spiro[4.5]decane (19 g) was obtained.

المصدر