反応 #67781

反応方程式

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

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

DIPEA

O-ethylhydroxylamine hydrochloride

→

desired product

収率 53.0%

N-Ethoxy-3-[(4-iodo-2-methylphenyl)amino]isonicotinamide

収率 53.0%

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 preparative reversed phase HPLC

実験手順

3-[(4-iodo-2-methylphenyl)amino]isonicotinic acid 2c (60 mg, 0.17 mmol) was dissolved in 6 ml dry DMF followed by the addition of DIPEA (0.20 mmol, 37 μl), ByBOP (0.20 mmol, 107 mg) and O-ethylhydroxylamine hydrochloride (0.34 mmol, 34 mg). The mixture was stirred for 4 h and the volatiles were removed in vacuo. The crude material was purified by preparative reversed phase HPLC to give 36 mg (91 μmol; 53% yield) of pure desired product.

出典