反应详情

温度

100 °C

A solution of dimethyl 5-(4-chlorobutanamido)isophthalate (0.635 g, 2.02 mmol, 1 eq) dissolved in 5 ml anhydrous DMF was added dropwise to a stirred suspension of NaH (60% dispersion in oil, 0.101 g, 2.53 mmol, 1.25 eq) in 2 ml anhydrous DMF at 0° C. under Ar. The reaction was stirred at 0° C. to room temperature overnight. After stirring overnight the reaction was heated to 100° C. for 19 h. After cooling to room temperature the reaction was poured into ice-water to quench. The mixture was extracted with EtOAc (×1). The organic layer was washed with water (×4), brine (×1), and dried over Na2SO4. The inorganics were filtered off, and the solvent was removed in vacuo. Purification via flash chromatography yielded 0.3487 g (1.26 mmol, 62% yield) of the product.

1. stirringAfter stirring overnight the reaction
2. temperatureAfter cooling to room temperature the reaction
3. customto quench
4. extractionThe mixture was extracted with EtOAc (×1)
5. washThe organic layer was washed with water (×4), brine (×1)
6. dry with materialdried over Na2SO4
7. filtrationThe inorganics were filtered off
8. customthe solvent was removed in vacuo
9. customPurification via flash chromatography