反应详情

温度

0 °C

Dissolve 5-amino-6-fluoro-N-methyl-N-propyl-isophthalamic acid ethyl ester (0.162 g, 0.58 mmol) in dichloromethane (1.5 mL). Cool to 0° C. Add pyridine (51.2 μL, 0.63 mmol) and methanesulfonyl chloride (44.5 μL, 0.58 mmol) to the solution. Allow the reaction to warm to room temperature and stir for 2 days. Quench with water (10 mL) and extract with dichloromethane (2×30 mL). Combine the organic layers and wash with saturated aqueous sodium chloride (20 mL), dry (magnesium sulfate), concentrate and purify (silica gel chromatography, eluting with 40:60 ethyl acetate:dichloromethane) to give the title compound as a solid (157 mg, 76%).

1. customthe reaction
2. temperatureto warm to room temperature
3. customQuench with water (10 mL)
4. extractionextract with dichloromethane (2×30 mL)
5. washCombine the organic layers and wash with saturated aqueous sodium chloride (20 mL)
6. dry with materialdry (magnesium sulfate)
7. concentrationconcentrate
8. custompurify
9. wash(silica gel chromatography, eluting with 40:60 ethyl acetate:dichloromethane)