反应详情

温度

90 °C

A solution of 2-(cyclopropylamino)-N-(2-methoxy-4-methyl-3-pyridinyl)-3-pyridinecarboxamide (0.3 g, 1 mmol) in 2 mL of dry pyridine under an argon atmosphere was treated with 2.2 mL of a 1.0M solution of NaHMDS. The solution was then warmed to 90° C. for 6 h. Upon cooling, the mixture was partitioned between EtOAc and 0.5N HCl. The EtOAc layer was then washed further with 0.5N HCl, dried (MgSO4) and concentrated. The residue was purified by flash chromatography on silica gel (1:1 EtOAc:Hexanes) to give 5,11-dihydro-4-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one in 91% yield (0.24 g).

1. temperatureUpon cooling
2. customthe mixture was partitioned between EtOAc and 0.5N HCl
3. washThe EtOAc layer was then washed further with 0.5N HCl
4. dry with materialdried (MgSO4)
5. concentrationconcentrated
6. customThe residue was purified by flash chromatography on silica gel (1:1 EtOAc:Hexanes)