反应详情

Biguanide (1.01 g.) was stirred in dry dimethylformamide (15 ml.) and N-(6-bromo-5-oxohexyl)phthalimide (1.5 g.) added. The mixture was stirred for 3 hours, acetic acid (5 ml.) was then added and the total reaction mixture evaporated to dryness. The residue was dissolved in water (10 ml.) and extracted with ethyl acetate (5×20 ml.). The combined ethyl acetate extracts were evaporated to give a brown foam which was purified by column chromatography on silica gel using chloroform/methanol/ammonia (s.g. 0.880) 80:20:0.5 v/v/v. The appropriate fractions were evaporated to give 2-guanidino-4-(4-phthalimidobutyl)imidazole as a brown foam (0.3 g.).

1. customthe total reaction mixture
2. customevaporated to dryness
3. dissolutionThe residue was dissolved in water (10 ml.)
4. extractionextracted with ethyl acetate (5×20 ml.)
5. customThe combined ethyl acetate extracts were evaporated
6. customto give a brown foam which
7. customwas purified by column chromatography on silica gel
8. customThe appropriate fractions were evaporated