p-Toluenesulfonic acid monohydrate → 4-(R,S)-(t-butoxycarbonylamino)-3-oxo-1,2diazolidine p-toluenesulfonate salt
反応式
[C:1]([O:5][C:6]([NH:8][CH:9]1[CH2:13][NH:12][NH:11][C:10]1=[O:14])=[O:7])([CH3:4])([CH3:3])[CH3:2].O.[C:16]1([CH3:26])[CH:21]=[CH:20][C:19]([S:22]([OH:25])(=[O:24])=[O:23])=[CH:18][CH:17]=1>C(Cl)Cl>[C:16]1([CH3:26])[CH:17]=[CH:18][C:19]([S:22]([OH:25])(=[O:23])=[O:24])=[CH:20][CH:21]=1.[C:1]([O:5][C:6]([NH:8][CH:9]1[CH2:13][NH:12][NH:11][C:10]1=[O:14])=[O:7])([CH3:4])([CH3:2])[CH3:3]参加物
4
実験手順
4-(R,S)-(t-Butoxycarbonylamino)-3-oxo-1,2-diazolidine (1.7 g, 8.45 mmol) was slurried in methylene chloride (50 ml). p-Toluenesulfonic acid hydrate (1.6 g, 8.45 mmol) was added to the slurry. After 20 minutes the resultant solid material was collected then dried in vacuo for approximately 48 hours to yield 2.95 g of colorless 4-(R,S)-(t-butoxycarbonylamino)-3-oxo-1,2diazolidine p-toluenesulfonate salt: n.m.r. (90 MHz, DMSO-d6) δ 7.5 (d, 2, J=8), 7.1 (d, 2, J=8), 4.32 (m, 1), 3.9 (m, 1), 3.4 (m, 1) 2.3 (s, 3), 1.4 (s, 9); i.r. (KBr): 1742, 1704, 1537 cm-1.