反应详情

To a suspension of 0.037 g 2-(4-methoxy-7-morpholin-4-yl-benzothiazol-2-yl)-1,4,5,6,7,8-hexahydro-imidazo[4,5-d]azepine hydrochloride in 3 ml tetrahydrofurane were added at 0–4° C. 0.06 ml N-ethyldiisopropylamine and 0.007 ml acetylchloride. The mixture was refluxed for 17 hours, silicagel was added and the solvent was distilled off. The residue was transferred to a column prefilled with silicagel and was chromatographed with dichloromethane/methanol 96:4 to yield 0.028 g (74%) 1-[2-(4-methoxy-7-morpholin-4-yl-benzothiazol-2-yl)-4,5,7,8-tetrahydro-1H-imidazo[4,5-d]azepin-6-yl]-ethanone as yellow solid; M.p.: 195–197° C.; MS (ISP): m/e=428 (M+H+).

1. additionwere added at 0–4° C
2. temperatureThe mixture was refluxed for 17 hours
3. additionsilicagel was added
4. distillationthe solvent was distilled off
5. customwas chromatographed with dichloromethane/methanol 96:4