3-methyl-2-nitrobenzamide synthesis
- Product Name:3-methyl-2-nitrobenzamide
- CAS Number:60310-07-8
- Molecular formula:C8H8N2O3
- Molecular Weight:180.16
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Yield:60310-07-8 95%
Reaction Conditions:
with ammonia;triethylamine in tetrahydrofuran;chloroformic acid ethyl ester;
Steps:
1.b b.
b. 3-Methyl-2-nitrobenzenecarboxamide To a solution of 3-methyl-2-nitrobenzoic acid (13.2 g) in tetrahydrofuran (150 ml) was added slowly at ambient temperature triethylamine (11.0 ml). After stirring for 30 minutes, the solution was cooled in an ice bath and ethyl chloroformate (7.6 ml) was added dropwise. Following the addition the thick mixture was stirred for 1 hour while maintaining the temperature at about 0°. Next, gaseous ammonia was bubbled through the well stirred mixture until it was well saturated (about 15 minutes). The cooling bath was removed and the mixture was allowed to warm slowly to ambient temperature with stirring for 2 hours. The mixture was partitioned between ethyl acetate and water; some gentle warming was required to solubilize all of the solid material. The layers were separated; the organic phase was washed with brine, dried over Na2 SO4 and concentrated to leave a white solid. Trituration with ether/hexane followed by filtration afforded the carboxamide (12.5 g, 95%); m.p. 189°-191°; tlc, Rf =0.08, silica gel, ethyl acetate:hexane (1:1).
References:
US4975435,1990,A
79-37-8
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99-04-7
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1885-77-4
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