反应详情

温度

-78 °C

Add bis(2-methoxyethyl) aminosulfur trifluoride (220 mg, 1.0 mmol) to a polypropylene tube (5 mL), seal, cool to −78° C., add a solution of 5-hydroxymethyl-N-methyl-N-propyl-isophthalamic acid ethyl ester (250 mg, 0.9 mmol) in dichloromethane (1 mL) in 0.2 mL increments. Stir at −78° C. for 3 h then at room temperature overnight. Pour the reaction into saturated aqueous sodium bicarbonate. Extract with dichloromethane, dry (magnesium sulfate), concentrate and purify (silica gel chromatography, eluting with 50:50 ethyl acetate:hexanes) to give the title compound (73 mg, 29%).

1. customseal
2. customat room temperature
3. customovernight
4. additionPour
5. extractionExtract with dichloromethane
6. dry with materialdry (magnesium sulfate)
7. concentrationconcentrate
8. custompurify
9. wash(silica gel chromatography, eluting with 50:50 ethyl acetate:hexanes)