Trifluoroacetic acid → (1S,9S)-9-(methoxycarbonylamino)-6,10-dioxooctahydro-1H-pyridazino[1,2-a][1,2]diazepine-1-carboxylic acid
反応式
[CH3:1][O:2][C:3]([NH:5][C@@H:6]1[C:12](=[O:13])[N:11]2[C@H:14]([C:18]([O:20]C(C)(C)C)=[O:19])[CH2:15][CH2:16][CH2:17][N:10]2[C:9](=[O:25])[CH2:8][CH2:7]1)=[O:4].FC(F)(F)C(O)=O>C(Cl)Cl>[CH3:1][O:2][C:3]([NH:5][C@@H:6]1[C:12](=[O:13])[N:11]2[C@H:14]([C:18]([OH:20])=[O:19])[CH2:15][CH2:16][CH2:17][N:10]2[C:9](=[O:25])[CH2:8][CH2:7]1)=[O:4]参加物
4
反応物 2
生成物 1
試薬・触媒・溶媒 1
実験手順
To a solution of (1S,9S)-tert-butyl 9-(methoxycarbonylamino)-6,10-dioxooctahydro-1H-pyridazino[1,2-a][1,2]diazepine-1-carboxylate (1.25 g, 3.52 mmol) dissolved into methylene chloride (10 mL) was added trifluoroacetic acid (10 mL). The reaction was stirred at room temperature for 1 h and concentrated in vacuo. Toluene (5 mL) was added and the reaction concentrated in vacuo to afford (1S,9S)-9-(methoxycarbonylamino)-6,10-dioxooctahydro-1H-pyridazino[1,2-a][1,2]diazepine-1-carboxylic acid as a white solid, (587 mg, 68%): ESI-LRMS m/e calcd for C12H17N3O6[M+] 299. found 300 [M+H+].