反应详情

温度

100 °C

A mixture of methyl 2-hydroxy-4-nitrobenzoate (1.1 g, 5.6 mmol), sodium 2-chloro-2,2-difluoroacetate (1.0 g, 6.6 mmol) and Na2CO3 (710 mg, 6.7 mmol) in DMF (10 mL) was stirred at 100° C. overnight. After cooling to rt, the mixture was partitioned between water and EtOAc. The organic layer was separated and washed with twice with water, then brine, dried over Na2SO4 and concentrated, and purified by a standard method to give the title product (330 mg). 1H NMR (CHLOROFORM-d) δ: 8.15-8.19 (m, 1H), 8.13 (s, 1H), 8.06 (d, J=8.6 Hz, 1H), 6.68 (s, 1H), 3.98 (t, J=72.8 Hz, 1H).

1. temperatureAfter cooling to rt
2. customthe mixture was partitioned between water and EtOAc
3. customThe organic layer was separated
4. washwashed with twice with water
5. dry with materialbrine, dried over Na2SO4
6. concentrationconcentrated
7. custompurified by a standard method