5-METHOXY-2-NITROBENZAMIDE synthesis
- Product Name:5-METHOXY-2-NITROBENZAMIDE
- CAS Number:41994-92-7
- Molecular formula:C8H8N2O4
- Molecular Weight:196.16
1882-69-5
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41994-92-7
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Yield:41994-92-7 80%
Reaction Conditions:
Stage #1: 5-methoxy-2-nitro-benzoic acidwith dichlorosulfoxide in N,N-dimethyl-formamide; for 1 h;Reflux;
Stage #2: with ammonia in lithium hydroxide monohydrate;N,N-dimethyl-formamide at 0;
Steps:
101.1
A 100 mL round bottom flask was charged with 5-methoxy-2- nitrobenzoic acid (1.5 g, 7.61 mmol), DMF (1 mL) and SOCl2 (15 mL). The resulting mixture was heated at reflux for 1 h then concentrated in vacuo. The residue was re-dissolved in DMF (3 mL) and the solution was added dropwise to aqueous ammonia (25%, 15 mL) at 0 °C with vigorous stirring. Work-up: the resulting solid was collected by filtration, washed with H20 (20 mL) and dried, to give 1.2 g (80%) of the product as white solid
References:
WO2011/112731,2011,A2 Location in patent:Page/Page column 143
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41994-92-7
11 suppliers
$45.00/100mg