反应详情

2.8 g (9.86 mmol) of 4-bromo-acetyl-2-methylimidazole hydrobromide was dissolved in 10 ml water. Saturated sodium bicarbonate solution was added to pH 10 and the resultant solid was collected by filtration and washed with 15 ml water. The dried free base was heated at reflux in 50 ml acetone. To the refluxing clear acetone solution was added 1.2 g (9.86 mmol) of amidinothiourea. Solution occurred immediately and within a minute a solid began to form. After one hour reflux the slurry was cooled and the solid was collected by filtration and was washed with acetone followed by ether to give 2.37 g (79%) of the title compound, M.P. 158° (dec.); nmr (DMSO-d6) (delta): 7.71 (s shoulder on broad s, 1H); 7.56 (broad s, 4H); 4.32 (s, 1H); 2.51 (s, 3H).

1. filtrationthe resultant solid was collected by filtration
2. washwashed with 15 ml water
3. temperatureThe dried free base was heated
4. temperatureat reflux in 50 ml acetone
5. customto form
6. temperatureAfter one hour reflux the slurry
7. temperaturewas cooled
8. filtrationthe solid was collected by filtration
9. washwas washed with acetone