反应详情

温度

60 °C

A mixture of 8-chloro-4-[3-(4-chloromethyl-thiazol-2-yl)-phenyl]-7-dimethylamino-1,3-dihydro-benzo[b][1,4]diazepin-2-one (89 mg) (Example 191a), morpholine (0.17 mL) and KI (3 mg) in EtOH (0.5 mL) was stirred at 60° C. for 3 h. H2O (25 mL) was added to the cooled solution and the precipitate was collected by filtration and purified by chromatography on silica gel using AcOEt/acetone (1:1) as eluent. The product was stirred with 20% aqueous MeOH (20 mL) The pH of the mixture was set to 11 by addition of 1N NaOH and the solid was subsequently isolated by filtration to give the title compound (55 mg) as yellow powder.

1. filtrationthe precipitate was collected by filtration
2. custompurified by chromatography on silica gel
3. stirringThe product was stirred with 20% aqueous MeOH (20 mL) The pH of the mixture
4. additionwas set to 11 by addition of 1N NaOH
5. customthe solid was subsequently isolated by filtration