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 (1L) 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 (1L)
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