反応 #45287

反応方程式

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

収率 100.8%

溶媒

THF

borane methyl sulfide

反応条件

後処理

1. 1
   温度After refluxing the reaction mixture for 12 h
2. 2
   温度the reaction was cooled
3. 3
   その他quenched with MeOH
4. 4
   その他After removal of THF
5. 5
   抽出the residue was extracted with ethyl acetate
6. 6
   洗浄washed with brine
7. 7
   乾燥dried with MgSO4
8. 8
   濃縮concentrated

実験手順

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.

出典