反応 #2504045

反応方程式

Carbonyldiimidazole

2-(2,4-difluoroanilino)-4,5-difluorobenzoic acid

O-Benzylhydroxylamine hydrochloride

triethylamine

→

title compound

収率 91.2%

N-Benzyloxy-2-(2,4-difluoroanilino)-4,5-difluoro-benzamide

収率 91.2%

溶媒

THF

反応条件

後処理

1. 1
   温度the mixture was heated
2. 2
   温度to reflux for 4 hours
3. 3
   濃縮The reaction mixture was concentrated
4. 4
   洗浄washed with 1N HCl, saturated NaHCO3, brine
5. 5
   乾燥dried over magnesium sulfate
6. 6
   濃縮The solution was concentrated

実験手順

Carbonyldiimidazole (3.1 g, 19.1 mmol) was added to a suspension of 2-(2,4-difluoroanilino)-4,5-difluorobenzoic acid (Example H-4, 4.54 g, 15.9 mmol) in 120 mL of THF, and the mixture was stirred for 24 hours at 25° C. O-Benzylhydroxylamine hydrochloride (2.54 g, 15.9 mmol) and triethylamine (2.66 mL, 19.1 mmol) were added, and the mixture was heated to reflux for 4 hours. The reaction mixture was concentrated and washed with 1N HCl, saturated NaHCO3, brine, and dried over magnesium sulfate. The solution was concentrated to give 5.66 g of the title compound as an oil.

出典