5,5-difluoro-2-oxo-piperidin-1-carboxylic acid t-butyl ester synthesis
- Product Name:5,5-difluoro-2-oxo-piperidin-1-carboxylic acid t-butyl ester
- CAS Number:911634-76-9
- Molecular formula:C10H15F2NO3
- Molecular Weight:235.23
911634-75-8
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911634-76-9
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Yield:911634-76-9 78%
Reaction Conditions:
with ruthenium(IV) oxide;sodium periodate in water;ethyl acetate at 20; for 21 h;
Steps:
12.2
0.53 g (2.5 mmol) of sodium methaperiodate (NaIO 4 ) was dissolved in 4 mL of water, and then 22 mg (0.17 mmol) of ruthenium oxide (RuO ) was added thereto. The resulting solution was dissolved in 7 mL of ethyl acetate. To this solution, 110 mg (0.5 mmol) of 3,3-difluoro-piperidin-l-carboxylic acid t-butyl ester obtained in the above step (1) was added, followed by stirring at room temperature for 21 hours. After stirring, the reaction solution was diluted by excess ethylacetate, and washed once with water and aqueous NaCl, respectively, and dried over anhydrous magnesium sulfate and filtered off. The filtrated solution was distilled off under reduced pressure, then the residue was purified by column chromatography (2:1 hexane: ethyl acetate) to give 91 mg of the title compound in a yield of 78%[504] 1K NMR (CDCl3) δ 3.97 (2H, t, J = 13 Hz), 2.66 (2H, t, J = 7.0 Hz), 2.3-2.4 (2H, m), 1.53 (9H, s)[505] Mass (m/e) 258 (M+Na)
References:
WO2006/104356,2006,A1 Location in patent:Page/Page column 35