反应详情

A stirred yellow suspension of 5-(2-diethylamino-ethyl)-2-(5-fluoro-2-oxo-1,2-dihydro-indol-3-ylidenemethyl)-3-methyl-1,5,6,7-tetrahydro-pyrrolo[3,2-c]pyridin-4-one (27 g, 66 mmol) in 600 ml of methanol was added with 2-hydroxyl-succinic acid (9.26 g, 69 mmol). The resulting solution was stirred for 30 minutes. The solvent was evaporated under reduced pressure and the residue was added with 100 ml of acetonitrile. The resulting solution was heated to reflux for 1.5 hours, cooled down to room temperature and filtered. The filter cake was washed with cold acetonitrile (100 ml×3) and ethanol (100 ml×3) and dried in vacuo to give the title compound 5-(2-diethylamino-ethyl)-2-(5-fluoro-2-oxo-1,2-dihydro-indol-3-ylidenemethyl)-3-methyl-1,5,6,7-tetrahydro-pyrrolo[3,2-c]pyridin-4-one malate (35 g, 95%) as a yellow solid.

1. customThe solvent was evaporated under reduced pressure
2. additionthe residue was added with 100 ml of acetonitrile
3. temperatureThe resulting solution was heated
4. temperatureto reflux for 1.5 hours
5. filtrationfiltered
6. washThe filter cake was washed with cold acetonitrile (100 ml×3) and ethanol (100 ml×3)
7. customdried in vacuo