反应详情

To a suspension of potassium carbonate (0.269 g, 1.949 mmol) in dry THF (5 mL) was added a THF solution (10 mL) of {3-[(3,5-bis-trifluoromethyl-benzylamino)-methyl]-5,6,7,8-tetrahydro-quinolin-2-yl}-cyclopentylmethyl-ethylamine (0.25 g, 0.3 mmol), which was then stirred for 1 h. Methylchloroformate (0.137 g, 1.46 mmol) was then added and stirring was was continued at RT for 8 h. The solvent was then evaporated, water was added, and the product was extracted with ethyl acetate. The organic layer was dried over sodium sulfate and the solvent was evaporated to afford a residue. This crude residue was purified over silica gel (100-200 mesh) and eluted with 2% ethyl acetate and petroleum ether to afford (3,5-bis-trifluoromethyl-benzyl)-[2-(cyclopentylmethyl-ethyl-amino)-5,6,7,8-tetrahydro-quinolin-3-ylmethyl]-carbamic acid methyl ester as light green, pasty compound (0.05 g, yield: 15%).

1. stirringstirring
2. waitwas was continued at RT for 8 h
3. customThe solvent was then evaporated
4. additionwater was added
5. extractionthe product was extracted with ethyl acetate
6. dry with materialThe organic layer was dried over sodium sulfate
7. customthe solvent was evaporated
8. customto afford a residue
9. customThis crude residue was purified over silica gel (100-200 mesh)
10. washeluted with 2% ethyl acetate and petroleum ether