A process for preparing anthranilic diamides and intermediates thereof
A technology of o-formamidobenzamide and compounds, which is applied in the field of preparation of o-formamidobenzamide compounds, and can solve problems such as laborious methods and lack of selectivity
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[0100] Step A: Preparation of 2-(hydroxyimino)-N-(o-tolyl)acetamide
[0101] To a solution of o-toluidine (75 g, 700 mmol) in water (170 mL) was slowly added hydrochloric acid (73 g, 700 mmol, 35% w / w), followed by anhydrous sodium sulfate (636 g, 4478 mmol) in water (800 mL). The resulting reaction mixture was heated to 55 °C. An aqueous solution of hydroxylamine hydrochloride (73 g, 1050 mmol) in water (280 mL) was then added slowly, followed by a solution of chloral hydrate (125 g, 757 mmol) in water (270 mL). The reaction mixture was maintained at 55°C for 12 hours. After the reaction was complete, the reaction mixture was cooled to 20 °C and stirred for 1 hour. The solid product was filtered and washed twice with water (100 mL) to give 2-(hydroxyimino)-N-(o-tolyl)acetamide (95 g, 531 mmol, yield: 76%).
[0102] 1 H-NMR (400MHz, DMSO-d 6 )δ12.16(s,1H),9.47(bs,1H),7.66(s,1H),7.45-7.47(d,J=7.8Hz,1H),7.19-7.24(dd,J=7.4Hz&0.6Hz ,1H),7.14-7.18(td,J=7.6Hz&1.6Hz,1H),7.08-7....
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