反応 #1568067

反応方程式

5-Bromo-2-nitrophenol

methyl 2-chloro-2,2-difluoroacetate

Potassium carbonate

→

title compound

収率 30.5%

2-(Difluoromethoxy)-4-bromo-1-nitrobenzene

収率 30.5%

溶媒

DMF

ethyl acetate

反応条件

後処理

1. 1
   温度The reaction was cooled to room temperature
2. 2
   洗浄The organic solution was washed with water (20 mL), brine (20 mL)
3. 3
   乾燥dried over sodium sulphate
4. 4
   濃縮concentrated in vacuo
5. 5
   その他The residue was purified by silica gel column chromatography
6. 6
   洗浄eluting with 20% dichloromethane in hexanes

実験手順

5-Bromo-2-nitrophenol (1 g, 4.59 mmol) and methyl 2-chloro-2,2-difluoroacetate (991 mg, 6.9 mmol) were dissolved in dry DMF (3 mL). Potassium carbonate (1.27 g, 9.18 mmol) was added and the reaction was stirred at 120° C. for 1 hour. The reaction was cooled to room temperature and diluted with ethyl acetate (20 mL). The organic solution was washed with water (20 mL), brine (20 mL), dried over sodium sulphate and concentrated in vacuo. The residue was purified by silica gel column chromatography eluting with 20% dichloromethane in hexanes to afford the title compound as a dark brown oil (375 mg, 30%).

出典