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CAS No. : | 18595-16-9 | MDL No. : | MFCD00661547 |
Formula : | C9H11NO2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | MDHYFUPTSWXVIA-UHFFFAOYSA-N |
M.W : | 165.19 | Pubchem ID : | 1201104 |
Synonyms : |
|
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 |
---|---|---|
60% | With ammonium chloride; zinc; In methanol; water; at 0 - 20℃; for 12.0h; | A solution of <strong>[20587-30-8]methyl 5-methyl-2-nitrobenzoate</strong> (8 g, 41.025 mmol) in methanol (80 mL) and water (10 mL) was cooled to 0C. Zinc powder (13.33 g, 205.128 mmol) was then added, followed by NH4C1 (17.6 g, 328.2 mmol). The mixture was stirred for 12 h at rt. Progress of the reaction was followed by TLC (20% ethyl acetate/hexane). After completion of the reaction, the mixture was filtered and the filtrate was evaporated to provide crude residue. The crude reside was basified with saturated NaHC03 solution and extracted with DCM (2 x 20 mL). The combined organic layers were dried over Na2S04, filtered and evaporated to give methyl 2-amino-5-methylbenzoate (Yield: 4 g, 60%).1H NMR (400 MHz, CDC13): delta 7.65 (s, 1H), 7.25 (s, 1H), 7.10-7.07 (q, 1H, J=8 Hz), 6.58 (d, 1H), 3.86 (s, 3H), 2.22 (s, 3H). |
With hydrogen;5% palladium-on-charcoal; In ethyl acetate; for 8.0h; | A mixture of which under argon gas 5% palladium carbon (1.55g) has been added to the compound (5.85g) prepared in Reference example 13, which ethyl acetate (150ml) had been added, was stirred for 8 hours under hydrate gas. The reactive mixture filtered with celite was concentrated. A title compound (4.89g) having the following physical properties values was obtained. TLC:Rf 0.44 (n-hexane: ethyl acetate =6:1); NMR (CDCl3):delta 7.66 (dd, J = 1.8 Hz, 0.6 Hz, 1H), 7.10 (m, 1H), 6.59 (d, J = 8.7 Hz, 1H), 5.56 (bs, 1H), 3.86 (s, 3H), 2.23 (s, 3H) |
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