반응 #420230

반응 방정식

Ethyl 2,2,3,3,3-pentafluoropropionate

Sodium borohydride

hydrochloric acid

→

1-Ethoxy-2,2,3,3,3-pentafluoro-propan-1-ol

용매

methanol

반응 조건

후처리

1. 1
   workup.ADDITIONAfter the addition
2. 2
   기타was held below −45° C
3. 3
   온도The mixture was cooled to −60° C.
4. 4
   기타remained below −45° C
5. 5
   온도The mixture was slowly warmed to room temperature
6. 6
   추출extracted with diethylether (3×100 ml)
7. 7
   세척The combined organic phases were washed with water (two times)
8. 8
   건조dried over magnesium sulfate
9. 9
   기타the solvent was removed under reduced pressure
10. 10
    기타9.76 g (50.3 mmol, 88%) were obtained

실험 절차

Ethyl 2,2,3,3,3-pentafluoropropionate (10.99 grams, 57.2 mmol) was dissolved in anhydrous methanol (57 ml) and cooled under argon to −60° C. Sodium borohydride (2.16 grams, 57.2 mmol) was added in four portions. After the addition was complete, stirring was continued for one hour and the temperature was held below −45° C. The mixture was cooled to −60° C. and 1M hydrochloric acid (172 ml) was added dropwise so that the temperature remained below −45° C. The mixture was slowly warmed to room temperature and extracted with diethylether (3×100 ml). The combined organic phases were washed with water (two times), dried over magnesium sulfate, the solvent was removed under reduced pressure. 9.76 g (50.3 mmol, 88%) were obtained and used directly in the next step.

출처