Реакция #45287

Уравнение реакции

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

Выход 100.8%

Растворители

THF

borane methyl sulfide

Условия реакции

Обработка

1. 1
   ТемператураAfter refluxing the reaction mixture for 12 h
2. 2
   Температураthe reaction was cooled
3. 3
   Другоеquenched with MeOH
4. 4
   ДругоеAfter removal of THF
5. 5
   Экстракцияthe residue was extracted with ethyl acetate
6. 6
   Промывкаwashed with brine
7. 7
   Сушкаdried with MgSO4
8. 8
   Концентрированиеconcentrated

Методика

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.

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