3-ethynyl-3-hydroxy-1-methyl-2-Piperidinone synthesis
- Product Name:3-ethynyl-3-hydroxy-1-methyl-2-Piperidinone
- CAS Number:1394119-72-2
- Molecular formula:C8H11NO2
- Molecular Weight:153.18
30932-82-2
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1394119-72-2
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Yield:1394119-72-2 30%
Reaction Conditions:
in tetrahydrofuran at -20 - 20; for 2.01667 h;Inert atmosphere;
Steps:
28.6 Step 6-Synthesis of 3-ethynyl-3-hydroxy-1-methylpiperidin-2-one
Step 6-Synthesis of 3-ethynyl-3-hydroxy-1-methylpiperidin-2-one To a solution of ethynylmagnesium bromide (0.5M in tetrahydrofuran, 4 mL, 2 mmol) maintained under nitrogen at -20° C. was added a solution of 1-methylpiperidine-2,3-dione (220 mg, 0.87 mmol) in tetrahydrofuran (3 mL) dropwise with stirring within 1 min. The reaction mixture was stirred for 2 hr at room temperature and then quenched by the addition of saturated ammonium chloride solution (1 mL). The mixture was diluted with DCM (50 mL), dried over anhydrous sodium sulfate and concentrated under vacuum. The crude residue was purified on a silica gel column, elution with ethyl acetate/petroleum ether (0:1-1:0) afforded the title compound (40 mg, 30%) as a brown oil: 1H NMR (400 MHz, CDCl3) delta 4.23 (s, 1H), 3.35-3.30 (m, 2H), 2.95 (s, 3H), 2.47 (s, 1H), 2.35-2.16 (m, 2H), 1.97-1.90 (m, 2H). LC-MS m/z=+154 [M+H]+.
References:
US2012/214762,2012,A1 Location in patent:Page/Page column 94
19365-01-6
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16867-04-2
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