反应详情

温度

80 °C

Methyl 2-(3-fluoro-4-hydroxyphenyl)acetate (prepared in Step A; 163 mg, 0.885 mmol) was diluted with DMSO (3 mL) followed by the addition of K2CO3 (122 mg, 0.885 mmol) and N-(4-chlorophenethyl)-4-chloro-3-nitrobenzamide (prepared in Step B; 300 mg, 0.885 mmol). The reaction was stirred at 80° C. for 12 hours. The reaction was cooled, diluted with DCM and washed with 10% aq. sodium carbonate, water and brine. The layers were separated and the organic layer was dried over MgSO4, filtered and concentrated. The material was purified by silica gel chromatography, eluting with hexane:acetone (2:1) to yield methyl 2-(4-(4-((4-chlorophenethyl)carbamoyl)-2-nitrophenoxy)-3-fluorophenyl)acetate (200 mg, 46.4% yield).

1. temperatureThe reaction was cooled
2. washwashed with 10% aq. sodium carbonate, water and brine
3. customThe layers were separated
4. dry with materialthe organic layer was dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe material was purified by silica gel chromatography
8. washeluting with hexane:acetone (2:1)