反应详情

A mixture of the disodium salt of 4-(3,5-dichlorophenyl)-[1,2,4]triazolidine-3,5-dione (7.65 g, 26.4 mmol) (Preparation 4) and 1,3-dibromo-2-(tert-butyldimethylsilyloxy)propane [11.7 g, 35.2 mmol; prepared according to Axenrod, et al. J. Org. Chem., Vol. 60 (1995), at pp. 1959-64] in DMF (160 ml) was heated under reflux for 2 h 45 min. The solvent was then removed under vacuum, and the resulting solid was chromatographed over silica gel (CH2Cl2) to yield the above compound as a white solid (2 g, mp=129° C.). 1H NMR (CDCl3): 7.51 (2H, m), 7.35 (1H, m), 4.52 (1H, br s), 3.95 (2H, d, J=11.6 Hz), 3.49 (2H, dd, J1=11.6 Hz, J2 =2 Hz), 0.81 (9H, s), 0.09 (6H, s).

1. customprepared
2. temperatureunder reflux for 2 h 45 min
3. customThe solvent was then removed under vacuum
4. customthe resulting solid was chromatographed over silica gel (CH2Cl2)