2,4-Dichloro-5-nitro-benzoic acid Methyl ester synthesis
- Product Name:2,4-Dichloro-5-nitro-benzoic acid Methyl ester
- CAS Number:101495-62-9
- Molecular formula:C8H5Cl2NO4
- Molecular Weight:250.04
35112-28-8
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Yield:101495-62-9 95%
Reaction Conditions:
with sulfuric acid;nitric acid at 0 - 20; for 18 h;
Steps:
Intermediate Q: Methyl 2,4-dichloro-5-nitrobenzoate
To a flask of methyl 2,4-dichlorobenzoate (500.0 mg, 2.44 mmol) at 0 00 was added conc. sulfuric acid (2.73 mL, 51.2 mmol) and then conc. nitric acid (0.46 mL, 9.27 mmol) in a drop-wise manner. The reaction was allowed to warm to r.t. and to proceed for 18 h. The reaction mixture was carefully poured into a flask of stirred ice water (100 mL). Once the ice had melted, EtOAc (40 mL) and sat. brine (20 mL) were then added and the layers separated. The aqueous layer was re-extracted with 3 x 10 mL EtOAc washings and the combined organics were then dried with Na2SO4 and concentrated under reduced pressure to afford the title compound as a yellow solid (579.2 mg, 95%). 1H NMR OH (ODd3, 500 MHz) 7.75 (d, J = 6.5 Hz, 1H), 7.42 (d, J = 8.8 Hz, 1H), 6.37 (5, 1 H), 4.86 (5, 1H), 4.72-4.57 (m, 1 H), 3.57 (5, 3H), 3.44-3.33 (m, 2H), 3.25-3.13 (m, 2H), 2.74 (dd, J = 14.2, 6.7 Hz, 2H).
References:
WO2018/122559,2018,A1 Location in patent:Page/Page column 37
67-56-1
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19861-62-2
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50-84-0
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