反应详情

8-(Benzyloxy)-5-(4-(4-(tert-butoxycarbonylamino)butyl)piperazin-1-yl)-1,6-naphthyridine-7-carboxylic acid (Example 4.2; 1.4 mmol) was dissolved in dichloro methane (14 ml). DIPEA (5.4 mmol) and HBTU (1.6 mmol) were added. The reaction mixture was stirred at room temperature during 5 min. Ethyl 2-(aminomethyl)-5-fluorobenzoate hydrochloride (Example 4; 1.6 mmol) was added portionwise at room temperature. The mixture was stirred overnight at room temperature. The mixture was diluted with CH2Cl2 and washed with a saturated aqueous Na2CO3 solution (2×) and H2O. The organic layer was separated, dried (MgSO4), filtered and evaporated. The residue was purified by flash column chromatography over silica gel (eluent: hexane/EtOAc 10:1 up to 1:1) to afford 0.97 gr of the title compound.

1. stirringThe mixture was stirred overnight at room temperature
2. washwashed with a saturated aqueous Na2CO3 solution (2×) and H2O
3. customThe organic layer was separated
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customevaporated
7. customThe residue was purified by flash column chromatography over silica gel (eluent: hexane/EtOAc 10:1 up to 1:1)