反应详情

Sodium hydride (14 mg, 0.34 mmol) was added to a solution of 3-[2-methyl-4-(3-methyl-4,10-dihydro-3H-2,3,4,9-tetraaza-benzo[f]azulene-9-carbonyl)-phenyl]-propionic acid tert-butyl ester from Example E45 (125 mg, 0.28 mmol) in DMF (2 ml) at 0° C. The mixture was stirred for 20 min at room temperature then cooled down to 0° C. Methyl iodide (0.09 ml, 1.4 mmol) was added and the mixture was stirred for 20 h at room temperature. EtOAc was added and the mixture was washed with 0.3M KHSO4 then brine, dried, concentrated in vacuo and azeotroped with toluene. The residue was purified by flash chromatography on silica gel through an isolute (eluant; EtOAc) to yield the title compound (46 mg, 36%).

1. temperaturethen cooled down to 0° C
2. stirringthe mixture was stirred for 20 h at room temperature
3. washthe mixture was washed with 0.3M KHSO4
4. dry with materialbrine, dried
5. concentrationconcentrated in vacuo
6. customazeotroped with toluene
7. customThe residue was purified by flash chromatography on silica gel through an isolute (eluant; EtOAc)