反应详情

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.

1. temperatureAfter refluxing the reaction mixture for 12 h
2. temperaturethe reaction was cooled
3. customquenched with MeOH
4. customAfter removal of THF
5. extractionthe residue was extracted with ethyl acetate
6. washwashed with brine
7. dry with materialdried with MgSO4
8. concentrationconcentrated