반응 #67780

반응 방정식

3-[(4-Bromo-2-methylphenyl)amino]isonicotinic acid

DIPEA

O-ethylhydroxylamine hydrochloride

→

desired product

수율 77.0%

3-[(4-Bromo-2-methylphenyl)amino]-N-ethoxyisonicotinamide

수율 77.0%

용매

DMF

반응 조건

후처리

1. 1
   기타the volatiles were removed in vacuo
2. 2
   기타The crude material was purified by flash chromatography

실험 절차

3-[(4-Bromo-2-methylphenyl)amino]isonicotinic acid 2b (320 mg, 1.04 mmol) was dissolved in 15 ml dry DMF followed by the addition of DIPEA (2.08 mmol, 373 μl), ByBOP (1.25 mmol, 651 mg) and O-ethylhydroxylamine hydrochloride (2.08 mmol, 203 mg). The mixture was stirred for 2 h and the volatiles were removed in vacuo. The crude material was purified by flash chromatography using silica gel and a gradient of 0-5% methanol in DCM as eluent to give 280 mg (800 μmol; 77% yield) of pure desired product.

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