反应详情

温度

50 °C

(Methoxycarbonylsulfamoyl)triethylammonium hydroxide, inner salt (179.7 mg, 0.754 mmol) was added to a solution of tert-butyl 4-[4-(aminocarbonyl)-2-oxo-2,3-dihydro-1H-imidazol-1-yl]piperidine-1-carboxylate (78 mg, 0.251 mmol) in dichloroethane (5 mL) and was heated to 50° C. After 1 h, the reaction was worked up with dichloromethane and saturated sodium bicarbonate. The organic extracts were washed with brine, dried over sodium sulfate, filtered and concentrated. Purification by silica gel chromatography (100% dichloromethane→5% methanol {1% ammonium hydroxide}/dichloromethane) gave the title compound (40 mg). MS 237.04 (M+1-tert butyl)

1. washThe organic extracts were washed with brine
2. dry with materialdried over sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated
5. customPurification by silica gel chromatography (100% dichloromethane→5% methanol {1% ammonium hydroxide}/dichloromethane)