反应详情

PBr3 (64.5 g, 22.5 mL, 0.239 mole) was added dropwise to a stirred, ice cold suspension of 4-hydroxy-6-methoxy-quinoline-3-carboxylic acid ethyl ester (59 g, 0.239 mole) in DMF (750 mL); the temperature rose to 15-20° C. for 30 min and then dropped to ca. 5° C. (the starting material dissolved fairly quickly and a new solid precipitated out). After 3 hr the solid was collected, washed sequentially with cold DMF, hexane, and water, then was dried at 40° C. in vacuo overnight to give the title compound (41 g, 78%): LC/MS (ES) m/e 310/312 (M+H)+.

1. additiondropped to ca. 5° C. (the starting material
2. dissolutiondissolved fairly quickly
3. customa new solid precipitated out)
4. customAfter 3 hr the solid was collected
5. washwashed sequentially with cold DMF, hexane, and water
6. customwas dried at 40° C. in vacuo overnight