Acetonitrile → HCID 68456140、化合物
反応式
Cl.[NH2:2][C:3]1[CH:10]=[CH:9][C:6]([CH2:7][NH2:8])=[CH:5][C:4]=1[F:11].C1([O:18][C:19](=O)[NH:20][CH2:21][C:22]2[CH:27]=[CH:26][C:25]([C:28]([CH3:31])([CH3:30])[CH3:29])=[CH:24][CH:23]=2)C=CC=CC=1.C(#N)C>C(N(CC)CC)C>[NH2:2][C:3]1[CH:10]=[CH:9][C:6]([CH2:7][NH:8][C:19]([NH:20][CH2:21][C:22]2[CH:27]=[CH:26][C:25]([C:28]([CH3:31])([CH3:30])[CH3:29])=[CH:24][CH:23]=2)=[O:18])=[CH:5][C:4]=1[F:11]参加物
5
実験手順
To the 50 ml of round bottom flask were put 4-amino-3-fluorobenzylamine hydrochloride (0.46 g, 3.28 mmol) and 4-t-butylbenzylcarbamic acid phenyl ester (1.1 eq, 1.02 g). And to this mixture was poured 20 ml acetonitrile and added triethylamine (excess, 0.5 ml) and refluxed 12 hours. After confirming the completion of the reaction with TLC, the reaction mixture was extracted with ethylacetate, washed with 1N HCl solution. And the combined organic layer was dried over MgSO4, filtered and concentrated under reduced pressure. The obtained liquid was column-chromatographed (n-hexane/ethyl acetate=1/1).