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CAS No. : | 88382-99-4 | MDL No. : | MFCD29043339 |
Formula : | C12H17NO2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 207.27 | Pubchem ID : | - |
Synonyms : |
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Signal Word: | Class: | ||
Precautionary Statements: | UN#: | ||
Hazard Statements: | Packing Group: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
91% | With sodium hydride; In tetrahydrofuran; mineral oil; for 1.0h; | General procedure: To a suspension of NaH (60% in oil, 3.1g, 77.7mmol) in THF (300mL) was added compound (S)-3 (15.0g, 77.7mmol). After 1h, a solution of CH3I (7.26mL, 116.6mmol) in THF (100mL) was added drop wise and the reaction mixture was stirred at 0C overnight. The reaction was quenched with methanol, and concentrated under reduced pressure. The residue was purified by column chromatography (silica gel, CH2Cl2/CH3OH=50:1, v/v) to give compound (S)-4 (14.6g, 91%) as a white solid. Mp=89-91C; [alpha]D20 -29.7 (c1.20, CHCl3); 1H NMR (400MHz, DMSO-d6) delta 7.81 (d, J=8.4Hz, 1H), 7.27 (t, J=7.6Hz, 2H), 7.20-7.18 (m, 3H), 4.07-4.01 (m, 1H), 3.27-3.21 (m, 2H), 3.25 (s, 3H), 2.77 (dd, J=13.6, 5.6Hz, 1H), 2.64 (dd, J=13.6, 8.0Hz, 1H), 1.75 (s, 3H); 13C NMR (100MHz, DMSO-d6) delta 168.64, 138.81, 128.99 (2C), 128.10 (2C), 125.98, 73.35, 58.16, 49.77, 36.87, 22.62; HRMS calcd for C12H18NO2 [M+H]+ 208.1332, found 208.1341. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Ca.100% | With hydrogenchloride; In water; for 24.0h;Reflux; | General procedure: Compound (S)-4 (14.0g, 67.6mmol) was refluxed in 6N HCl (90mL) for 24h. The solvent was evaporated under reduced pressure to obtain compound (S)-5 (13.6g) as a white solid in an almost quantitative yield. Mp=122-124C; [alpha]D20 -13.3 (c 1.20, CH3OH); 1H NMR (400MHz, DMSO-d6) delta 8.45 (s, 2H), 7.34 (t,J=7.2Hz, 2H), 7.30-7.26 (m, 3H), 3.44-3.41 (m, 2H), 3.33 (dd, J=10.4, 6.0Hz, 1H), 3.27 (s, 3H), 3.08 (dd, J=13.2, 4.8Hz, 1H), 2.83 (dd, J=13.2, 9.2Hz, 1H), 2.59 (t, J=4.8Hz, 1H); 13C NMR (100MHz, DMSO-d6) delta 136.41, 129.17 (2C), 128.59 (2C), 126.79, 70.08, 58.43, 51.54, 34.91; HRMS calcd for C10H16NO [M+H]+ 166.1226, found 166.1227. |