PENTAFLUOROPROPIONALDEHYDE ETHYL HEMIACETAL synthesis
- Product Name:PENTAFLUOROPROPIONALDEHYDE ETHYL HEMIACETAL
- CAS Number:337-28-0
- Molecular formula:C5H7F5O2
- Molecular Weight:194.1
426-65-3
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Yield:337-28-0 88%
Reaction Conditions:
with methanol;sodium tetrahydroborate at -60 - -45; for 1 h;Inert atmosphere;
Steps:
2.A
Step A: 1-Ethoxy-2,2,3,3,3-pentafluoro-propan-1-ol; 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 1 M hydrochloric acid (172ml) was added dropwise so that the temperature remained below -45°C. The mixture was slowly warmed to room temperature and extracted with diethylether (3x100 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.
References:
WO2012/41873,2012,A1 Location in patent:Page/Page column 86
