2-Amino-3,4-dichlorobenzoicacid synthesis
- Product Name:2-Amino-3,4-dichlorobenzoicacid
- CAS Number:20776-62-9
- Molecular formula:C7H5Cl2NO2
- Molecular Weight:206.03
18711-12-1
20776-62-9
General procedure for the synthesis of 2-amino-3,4-dichlorobenzoic acid from 6,7-dichloroindole-2,3-dione: 6,7-dichloroindole-2,3-dione (1 g, 4.6 mmol) was added to an aqueous (10.5 mL) suspension of potassium hydroxide (370 mg, 6.6 mmol) and potassium chloride (920 mg, 12.3 mmol) cooled to 0 °C . Subsequently, a 30 wt% aqueous hydrogen peroxide solution (1.1 mL, 35 mmol) was added slowly and dropwise. The reaction mixture was stirred at room temperature for 30 min, then ethyl acetate (4.0 mL) was added. The resulting mixture was washed sequentially with water, the organic layer was separated and dried over anhydrous sodium sulfate. Decarboxylation product (910 mg, 95% yield) was obtained after concentration under reduced pressure. The structure of the product was confirmed by 1H NMR (400 MHz, DMSO-d6): δ 13.16 (s, 1H), 7.73 (d, J = 8.6 Hz, 1H), 7.11 (s, 2H), 6.81 (d, J = 8.6 Hz, 1H).
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Yield:20776-62-9 95%
Reaction Conditions:
with potassium chloride;water;dihydrogen peroxide;potassium hydroxide at 0 - 20; for 0.5 h;Inert atmosphere;
Steps:
A Stw A: 2-amino-3,4-dichlorobenzoic acid
To a cooed (0 C) suspension of potassium hydroxide (370 mg, 6.6 mmd) and potassum chorde (920 mg, 12.3 mmd) n water(10.5 mL) was added 67dchorondo ne2,3done (1 g, 4.6 mmd), foHowed by dropwse addtion of 30 wt% aqueous hydrogen peroxide (1.1 mL, 35 mmd). The resuWng mxture was stirred for 30 mnutes at rt, Acetic add (4.0 mL) was added and the resuWng yeflow predp[tate was ifitered, washed wth water and dried in vacuo to afford the desred product (910 rng, 95% yed). 1H NMR (400 MHz, DM50-cl6) 3 13.16(5, IH), 7.73 (d, J= 8.6 Hz, IH), 7.11 (s, 2H), 6.81 (d, J= 8.6 Hz, IH).
References:
WO2016/176449,2016,A1 Location in patent:Page/Page column 89
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