反应详情

A solution of [7-(4-t-butoxycarbonylpiperazin-1-yl)-3,4-dihydro-1(1H)-isoquinolinone-2-yl]acetic acid (1-5) (195 mg, 0.5 mmol), ethyl 3-amino-3(S)-(3-pyridyl)propionate dihydrochloride (1-6) (Rico et al, J. Org. Chem. 1993, vol. 58, p. 7948; 127 mg, 0.55 mmol), EDC (105 mg, 0.55 mmol), HOBT (74 mg, 0.55 mmol) and 4-methylmorpholine (0.12 mL, 1.1 mmol) in DMF (5 mL) was stirred at room temperature for 16 hours. The mixture was diluted with EtOAc and water and the pH adjusted to ~pH 7 with 1N LiOH. The solution was extracted with EtOAc (3×), dried (MgSO4) and the solvent removed in vacuo. Purification of the residue by column chromatography (10% MeOH in EtOAc) gave 1-7. Rf (silica, 10% MeOH in EtOAc)=0.43.

1. extractionThe solution was extracted with EtOAc (3×)
2. dry with materialdried (MgSO4)
3. customthe solvent removed in vacuo
4. customPurification of the residue by column chromatography (10% MeOH in EtOAc)
5. customgave 1-7