반응 #994783

반응 방정식

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

수율 100.8%

용매

THF

borane methyl sulfide

반응 조건

후처리

1. 1
   온도After refluxing the reaction mixture for 12 h
2. 2
   온도the reaction was cooled
3. 3
   기타quenched with MeOH
4. 4
   기타After removal of THF
5. 5
   추출the residue was extracted with ethyl acetate
6. 6
   세척washed with brine
7. 7
   건조dried with MgSO4
8. 8
   농축concentrated

실험 절차

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.

출처