C(OC(=O)[NH:7][CH2:8][CH2:9][N:10]1[CH:14]=[C:13]([I:15])[N:12]=[C:11]1[CH2:16][CH2:17][CH3:18])(C)(C)C.[ClH:20].O1CCOCC1>C(Cl)Cl>[I:15][C:13]1[N:12]=[C:11]([CH2:16][CH2:17][CH3:18])[N:10]([CH2:9][CH2:8][NH2:7])[CH:14]=1.[ClH:20]To an ice-cooled solution of [2-(4-iodo-2-propyl-imidazol-1-yl)-ethyl]-carbamic acid tert-butyl ester (6.110 g; 16.111 mmol) in DCM (100 ml) was added slowly 4N HCl in dioxane (80.5 ml; 322 mmol; 20 eq.). The resulting suspension was stirred at 0° C. for 15 min., and then at rt for 2 h. The volatiles were removed under reduced pressure, then under HV. The product 2-(4-iodo-2-propyl-imidazol-1-yl)-ethylamine was obtained as a colorless solid (5.620 g; 100%; presence of 2 eq. of HCl). LC-MS: tR=0.24 min.; [M+H]+=279.96 g/mol.
読み込み中…
