反应详情

Methyl iodide (1.4 ml) and sodium bicarbonate (630 mg) were added to a solution of 2-oxo-3-tert-butoxycarbonylamino-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine (832 mg) in methanol (20 ml), the mixture was refluxed for 2 days. The reaction mixture was concentrated under reduced pressure, Water (30 ml) was added to the residue and extracted with methylene chloride. The organic layer was washed with saturated brine, dried over anhydrous sodiun sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform:methanol=50:1), to thereby obtain 585 mg of the title compound (Yield: 66.9%) as brown amorphous.

1. temperaturethe mixture was refluxed for 2 days
2. concentrationThe reaction mixture was concentrated under reduced pressure, Water (30 ml)
3. additionwas added to the residue
4. extractionextracted with methylene chloride
5. washThe organic layer was washed with saturated brine
6. dry with materialdried over anhydrous sodiun sulfate
7. customthe solvent was evaporated under reduced pressure
8. customThe residue was purified by silica gel column chromatography (chloroform:methanol=50:1)