反应详情

温度

85 °C

A mixture of 921 mg (2.00 mmol) of 3-{1-[4-(3,4-dichloro-phenyl)-1,4-dioxobutyl]-4-piperidinyl}-3,4-dihydro-2(1H)-quinazolinone, 377 mg (2.2 mmol) of 1-(3-dimethylaminopropyl)-piperazine, 10 ml of DMSO and 0.276 g (2.00 mmol) of potassium carbonate was stirred for 24 hours at a reaction temperature of 85° C. The mixture was diluted with 200 ml of water, then extracted exhaustively with EE. The combined extracts were dried over sodium sulphate and concentrated by evaporation in vacuo. The residue remaining was purified twice by column chromatography on silica gel (Amicon, 35–70 μm) (dichloromethane/methanol/conc. ammonia 70/30/1 v/v/v as eluant). The appropriate eluates were combined and after working up in the usual way yielded 30.0 mg (2.5% of theoretical) of the desired substance as a colourless, amorphous substance. Rf 0.68 (El D) or 0.35 (eluant: dichloromethane/methanol/conc. ammonia 50/50/1 v/v/v). MS: M+594/596 (Cl); ESI: (M+H)+=595/597 (Cl)

1. extractionextracted exhaustively with EE
2. dry with materialThe combined extracts were dried over sodium sulphate
3. concentrationconcentrated by evaporation in vacuo
4. customThe residue remaining was purified twice by column chromatography on silica gel (Amicon, 35–70 μm) (dichloromethane/methanol/conc. ammonia 70/30/1 v/v/v as eluant)
5. customyielded 30.0 mg (2.5% of theoretical) of the desired substance as a colourless, amorphous substance