反应详情

To a solution of 4-chloro-N-{1-[(4-cyclobutyl-1,4-diazepan-1-yl)carbonyl]azetidin-3-yl}benzamide (15 mg, 38 μmol) in THF (2 ml) was added NaH (3 mg of a 60% dispersion in mineral oil, 76 μmol). The reaction was stirred at room temperature for 30 minutes and then MeI (2.6 μmol, 46 μmol) was added. The reaction was heated in a sealed tube at 50° C. for 3 hours and then concentrated at reduced pressure, diluted with dichloromethane (30 ml), washed twice with saturated NaHCO3 (15 ml), dried (MgSO4), filtered and concentrated at reduced pressure. The residue was purified by FCC (DCM/MeOH/NH3 with gradient, 95:5:1 to 90:10:1) to provide the title compound as colourless oil (10 mg, 66%).

1. temperatureThe reaction was heated in a sealed tube at 50° C. for 3 hours
2. concentrationconcentrated at reduced pressure
3. additiondiluted with dichloromethane (30 ml)
4. washwashed twice with saturated NaHCO3 (15 ml)
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated at reduced pressure
8. customThe residue was purified by FCC (DCM/MeOH/NH3 with gradient, 95:5:1 to 90:10:1)