反应详情

温度

85 °C

Into a 500 mL beaker, 1-(3-Benzoyl-thioureido)-4-bromo-1H-pyrrole-2-carboxylic acid methyl ester (31.20 g, 0.08162 mol) and 2.00 M of Sodium hydroxide in Water (164 mL, 0.327 mol) were added. The mixture was heated at 85° C. for 75 minutes. The reaction was cooled to RT. The solid was dissolved with Ethanol (100 mL). Acetic acid (18.8 mL, 0.332 mol) was added at 0° C. and stirred for 30 minutes. The solid was filtered and washed with cold EtOH (50 mL) to afford a white solid. The white solid was stirred in Et2O (300 mL) for 20 minutes. The solid was filtered and washed with Et2O (200 mL) to give 6-Bromo-2-thioxo-2,3-dihydro-1H-pyrrolo[2,1-f][1,2,4]triazin-4-one as a white solid. The white solid was dried under vacuum over night (11.6, 57%).

1. temperatureThe reaction was cooled to RT
2. filtrationThe solid was filtered
3. washwashed with cold EtOH (50 mL)
4. customto afford a white solid
5. filtrationThe solid was filtered
6. washwashed with Et2O (200 mL)