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11-[2-(4-methylpiperazin-1-yl)acetyl]-5,11-dihydro-6H-pyrido[2,3-b][1,4]benzodiazepin-6-thione[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
2.7 g (30%)
With diphosphorus pentasulfide; sodium hydrogencarbonate; In pyridine; methanol; chloroform;
EXAMPLE 6 11-[2-(4-Methylpiperazin-1-yl)acetyl]-5,11-dihydro-6H-pyrido[2,3-b][1,4]benzodiazepin-6-thione A suspension of <strong>[29868-97-1]11-[2-(4-methylpiperazin-1-yl)acetyl]-5,11-dihydro-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one dihydrochloride</strong> (10.6 g) and phosphorus pentasulfide (6.1 g) in pyridine (125 ml) was refluxed under stirring for 7 hours. After cooling and filtration, the collected solid was suspended in chloroform (500 ml) and the suspension was repeatedly washed with saturated solution of sodium bicarbonate until disappearance of solid in suspension. The organic phase was dried on sodium sulphate and evaporated. The residue, crystallized first from acetonitrile and then from methanol, yielded 2.7 g (30%) of 11-[2-(4-methylpiperazin-1-yl)acetyl]-5,11-dihydro-6H-pyrido[2,3-b][1,4]benzodiazepin-6-thione melting at 240-241 C.