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CAS No. : | 76045-71-1 | MDL No. : | MFCD06797571 |
Formula : | C7H7NO3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | QPEJHSFTZVMSJH-UHFFFAOYSA-N |
M.W : | 153.14 | Pubchem ID : | 127115 |
Synonyms : |
|
Chemical Name : | 3-Amino-5-hydroxybenzoic acid |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H315-H319-H335 | Packing Group: | N/A |
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 |
---|---|---|
With palladium on activated charcoal; hydrogen; In methanol; under 760.051 Torr; for 2h; | Compound 5C was dissolved in methanol (20 mL) and hydrogenated under normal pressure for 2 hours under Pd/C. The diatomaceous earth was filtered to remove Pd/C, and methanol was spun off to obtain a crude product of compound 8D, which was directly taken to the next step. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
90% | In acetonitrile; at 20℃; for 1h; | A mixture of <strong>[76045-71-1]3-amino-5-hydoxybenzoic acid</strong> (30.7 g, 200.7 MMOL) and benzoylisothiocyanate (26.57 g) in acetonitrile (450 mL) was stirred at room temperature for 1 h. The precipitate was filtered and washed with acetonitrile and dried to afford 57.17 g (90%) of the desired product as a YELLOW POWDER. 1H NMR (CD30D) 8 8.01-8. 04 (m, 2H), 7.79 (m, 1 H), 7.69 (m, 1 H), 7.58-7. 63 (m, 2H), 7.37 (m, 1H). ANAL. CALCD FOR C15H12N2SO4 : Mol. Wt, 316.0518. Found. 317.0593 (M+H, HRMS). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In DMF (N,N-dimethyl-formamide); | 3-Amino-5-hydroxybenzoic acid (2000 g, 13.07 moles) was dissolved in DIMETHYLFORMAMIDE (8 L) and then methyl isothiocyanate (954 g, 13.07 moles) was added and the reaction mixture was stirred overnight. This gave crude N- METHYL-N - (5-HYDROXY-3-CARBOXYPHENYL) thiourea in solution, which was used for the next reaction. 1H NMR (DMSOd6) 8 2. 95 (s, 3H), 7.08 (s, 1H), 7.19 (s, 1H), 7.37 (s, 1H), 7.78 (s, 1H), 9.63 (s, 1H), 9.78 (s, 1H), 12.85 (s, 1H). |
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