反应详情

A solution of 8a (1.83 g, 7.72 mmol) and N,N-dimethylethylenediamine (3.40 g, 38.6 mmol) in propan-1-ol (80 ml) was flushed with N2, and the mixture was heated at reflux for three days under N2. Solvent was then removed under reduced pressure, and the residue was partitioned between CH2Cl2 (100 ml) and 1M Na2CO3 (100 ml). The organic layer was evaporated and the residue chromatographed on alumina, eluting with CH2Cl2 /MeOH (199:1) to give N-[2-dimethylamino)ethyl]acridine-4-carboxamide 3a (1.38 g, 61%), mp (diHCl salt) 191-195° C., identical with an authentic sample.

1. temperaturethe mixture was heated
2. temperatureat reflux for three days under N2
3. customSolvent was then removed under reduced pressure
4. customthe residue was partitioned between CH2Cl2 (100 ml) and 1M Na2CO3 (100 ml)
5. customThe organic layer was evaporated
6. customthe residue chromatographed on alumina
7. washeluting with CH2Cl2 /MeOH (199:1)