反応 #67780

反応方程式

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

DIPEA

O-ethylhydroxylamine hydrochloride

→

desired product

収率 77.0%

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

収率 77.0%

溶媒

DMF

反応条件

後処理

1. 1
   その他the volatiles were removed in vacuo
2. 2
   その他The crude material was purified by flash chromatography

実験手順

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.

出典