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CAS No. : | 38116-61-9 | MDL No. : | MFCD00460503 |
Formula : | C7H7NO3 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | XRIHTJYXIHOBDQ-UHFFFAOYSA-N |
M.W : | 153.14 | Pubchem ID : | 94960 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P305+P351+P338 | UN#: | |
Hazard Statements: | H319 | Packing Group: | |
GHS Pictogram: |
* 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 |
---|---|---|
64.1% | With sulfuric acid; at 0℃; for 21h;Reflux; | To a solution of <strong>[38116-61-9]2-hydroxy-6-methylnicotinic acid</strong> (10.0 g, 0.0653 mole) in methanol (100 mL), sulfuric acid (3.5 mL) was added drop wise at 0 C and the mixture was stirred for 21 h under reflux. The reaction mixture was concentrated under reduced pressure, the residue was neutralized with saturated aqueous sodium bicarbonate solution under ice-cooling, and the mixture was extracted with 5 % methanol in chloroform (200 mL x 3). Organic layer was washed with brine solution (50 mL) and dried over Na2S04 and the solvent was concentrated under vacuum to afford the title compound. (0233) Yield: 7.0 g, 64.1%; 1H - NMR (DMSO- 6, 400 MHz) d ppm: 2.23 (s, 3H), 3.70 (s, 3H), 6.09 - 6.11 (d, J = 7.24 Hz, 1H), 7.98 - 8.00 (d, J = 7.36 Hz, 1H), 12.10 (s, 1H); Mass (m/z): 168.1 (M+H)+. |