反应详情

To (5,5-dimethyl-3-oxo-1-(2,4,6-trimethylbenzene-sulfonyl)piperazin-2-yl)acetic acid (0.32 g, 0.94 mmol) in DMF (3 mL) was added cycloheptyl amine (0.5 mL), EDC (0.5 g, 2.5 mmol), and DMAP (0.3 g, 2.6 mmol). The mixture was stirred at RT overnight. TLC indicated that the reaction was not complete. Additional EDC (0.3 g) was added and the mixture was heated at 65° C. for 1 h. The mixture was cooled to RT. EtOAc (80 mL) was added and mixture was washed with dilute HCl in brine. The EtOAc solution was dried and evaporated to give the crude compound. Column chromatograph purification (silica gel, 0-2% MeOH/CH2Cl2) gave the titled compound. MS: 464.1 (M+1)+.

1. temperaturethe mixture was heated at 65° C. for 1 h
2. temperatureThe mixture was cooled to RT
3. washmixture was washed with dilute HCl in brine
4. dry with materialThe EtOAc solution was dried
5. customevaporated
6. customto give the crude compound
7. customColumn chromatograph purification (silica gel, 0-2% MeOH/CH2Cl2)