反应详情

温度

80 °C

To a solution of 1-tert-butyl 3-methyl (3R*,5S*)-5-{[(2-tert-butyl-4-chloropyrimidin-5-yl)carbonyl](isobutyl)amino}piperidine-1,3-dicarboxylate (51.1% mg) and diisopropylethylamine (38 mg) in DMF (0.5 ml) was added a solution of 3-methylthiopropylamine (21 mg) in DMF (0.5 ml), and the mixture was stirred at 80° C. overnight. To the reaction mixture was added 2% aqueous sodium hydrogen carbonate and the mixture was extracted with ethyl acetate, and the extract was concentrated by a nitrogen gas blower. The residue was purified by reversed-phase preparative HPLC, and the object fraction was concentrated by a nitrogen gas blower. The residue was dissolved in trifluoroacetic acid/acetonitrile solution (20% (V/V), 1.0 ml), and the mixture was stirred at room temperature for 6 hr. The reaction mixture was concentrated by a nitrogen gas blower. The residue was neutralized with triethylamine (1 ml), saturated aqueous sodium hydrogen carbonate was added, and the mixture was extracted with ethyl acetate. The extract was concentrated by a nitrogen gas blower. The residue was purified by reversed-phase preparative HPLC, and the object fraction was concentrated by a nitrogen gas blower to give the object compound (6.4 mg).

1. extractionthe mixture was extracted with ethyl acetate
2. concentrationthe extract was concentrated by a nitrogen gas blower
3. customThe residue was purified by reversed-phase preparative HPLC
4. concentrationthe object fraction was concentrated by a nitrogen gas blower
5. dissolutionThe residue was dissolved in trifluoroacetic acid/acetonitrile solution (20% (V/V), 1.0 ml)
6. stirringthe mixture was stirred at room temperature for 6 hr
7. concentrationThe reaction mixture was concentrated by a nitrogen gas blower
8. additionwas added
9. extractionthe mixture was extracted with ethyl acetate
10. concentrationThe extract was concentrated by a nitrogen gas blower
11. customThe residue was purified by reversed-phase preparative HPLC
12. concentrationthe object fraction was concentrated by a nitrogen gas blower