反应详情

To a solution of 6-hydroxycarbostyril (1.6 g) and sodium hydride (50% oily) (1 g) in dimethylformamide (30 ml), 1-chloro-2-hydroxy-3-(N-methyl-N-benzylamino)propane (2.2 g) is added dropwise at room temperature. After the addition, the mixture is heated with stirring at 70°-80° C. for 3 hours. The reaction mixture is poured into water and extracted with chloroform, and the extract is dried over magnesium sulfate. Chloroform is distilled off and the resulting residue is purified by silica gel column chromatography (solvent; methanol:chloroform=1:100-1:25) and recrystallized from ethanol to give 6-[3-(N-methyl-N-benzylamino)-2-hydroxypropoxy]carbostyril (0.76 g), as white powder, m.p. 129°-132° C.

1. additionAfter the addition
2. temperaturethe mixture is heated
3. extractionextracted with chloroform
4. dry with materialthe extract is dried over magnesium sulfate
5. distillationChloroform is distilled off
6. customthe resulting residue is purified by silica gel column chromatography (solvent; methanol:chloroform=1:100-1:25)
7. customrecrystallized from ethanol