反应详情

温度

140 °C

4-Amino-2,3-difluoro-5-nitro-benzoic acid methyl ester 4 (1.50 g, 6.46 mmol) is suspended in xylenes (7.5 mL) and 2-fluoro-phenylamine (6.24 mL, 64.6 mmol) is added. The reaction mixture is stirred at 140° C. under N2. After stirring for 6 days, the reaction is complete. The reaction mixture is cooled to room temperature and diluted with methylene chloride and filtered through a silica gel plug eluting with methylene chloride (1 L) to give an orange filtrate. The filtrate is concentrated to dryness and then triturated with diethyl ether to yield a bright yellow solid. The trituration is repeated. The yellow solid is collected to yield 1.08 g (52%) of the pure desired product. MS APCI (−) m/z 322 (M−1) detected.

1. stirringAfter stirring for 6 days
2. temperatureThe reaction mixture is cooled to room temperature
3. filtrationfiltered through a silica gel plug
4. washeluting with methylene chloride (1 L)
5. customto give an orange filtrate
6. concentrationThe filtrate is concentrated to dryness
7. customtriturated with diethyl ether
8. customto yield a bright yellow solid
9. customThe yellow solid is collected