Triethyl 2,2',2''-(1,4,7,10-tetraazacyclododecane-1,4,7-triyl)triacetate → HCID 67600478、化合物
反応式
[CH2:1]([O:3][C:4]([CH2:6][N:7]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14][N:13]([CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])[CH2:12][CH2:11][N:10]([CH2:25][C:26]([O:28][CH2:29][CH3:30])=[O:27])[CH2:9][CH2:8]1)=[O:5])[CH3:2].[C:31]1([CH2:37][CH2:38][N:39]([CH2:44][CH:45]2[CH2:47][O:46]2)[S:40]([CH3:43])(=[O:42])=[O:41])[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1>C(O)C>[C:31]1([CH2:37][CH2:38][N:39]([S:40]([CH3:43])(=[O:42])=[O:41])[CH2:44][CH:45]([OH:46])[CH2:47][N:16]2[CH2:15][CH2:14][N:13]([CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])[CH2:12][CH2:11][N:10]([CH2:25][C:26]([O:28][CH2:29][CH3:30])=[O:27])[CH2:9][CH2:8][N:7]([CH2:6][C:4]([O:3][CH2:1][CH3:2])=[O:5])[CH2:18][CH2:17]2)[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1参加物
4
実験手順
200 ml of absolute ethanol is poured over 8.61 g (20 mmol) of N,N',N"-tris-(ethoxycarbonylmethyl)-1,4,7,10-tetraazacyclododecane (produced according to DE 36 25 417 A1) in a bomb tube. After 5.11 g (20 mmol) of N-(2-phenylethyl)-N-[(2-oxiranyl)-methyl]-methanesulfonic acid amide is added (Example 2f), the bomb tube is closed, flushed with nitrogen, and the resulting reaction mixture is heated for 16 hours to 90° C. After the reaction (TLC control) is completed, the solvent is evaporated in a vacuum and the yellowish, oily residue is chromatographed on silica gel (Eluent: chloroform/methanol; methanol: 0-80%).