[C:1]1([CH:7]([C:12]2[CH:17]=[CH:16][N:15]=[N:14][CH:13]=2)[CH2:8][C:9](O)=[O:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CCN(CC)CC.C1C=CC(P([N:39]=[N+:40]=[N-:41])(C2C=CC=CC=2)=O)=CC=1>CN(C=O)C.O>[C:1]1([CH:7]([C:12]2[CH:17]=[CH:16][N:15]=[N:14][CH:13]=2)[CH2:8][C:9]([N:39]=[N+:40]=[N-:41])=[O:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1To a solution of 3-phenyl-3-(pyridazin-4-yl)propanoic acid (570 mg, 2.5 mmol) in DMF (30 mL) was added Et3N (505 mg, 5.0 mmol), followed by the DPPA (722 mg, 2.6 mmol) in portions at 0° C., the resulting mixture was stirred at room temperature for 1.5 hour. The reaction was diluted with water, extracted with AcOEt (3×40 ml), the combined organic layer was washed by brine, dried over Na2SO4 and concentrated to get the 3-phenyl-3-(pyridazin-4-yl)propanoyl azide (crude 650 mg), which was used for next step directly.
Wird geladen…
