反应详情

A suspension of 4-hydroxy-6-methyl-1,3,3a,7-tetraazaindene (15.0 g, 0.1 mol) in acetic acid (100 ml) was treated dropwise at 20° C. with a solution of bromine (16.172 g, 0.102 mol) in acetic acid (20 ml). As the reaction progressed, the suspended crystals dissolved and new crystals of brominated product were formed. After about 2 hours, the reaction mixture was poured into water (250 ml) and crystals were collected by filtration. The crude product was purified by first converting into its sodium salt by dissolving 22 g in one liter of hot aqueous 0.2N sodium carbonate and then slowly acidifying with dilute hydrochloric acid. The unchanged starting material was converted into a soluble salt by addition of excess of triethylamine. Crystals were then collected and recrystallized from hot water to give 19 g (82%) of Compound TAI-4 as white needles, m.p.=269° C.

1. dissolutionthe suspended crystals dissolved
2. customnew crystals of brominated product were formed
3. filtrationwere collected by filtration
4. customThe crude product was purified
5. dissolutionby dissolving 22 g in one liter of hot aqueous 0.2N sodium carbonate
6. additionwas converted into a soluble salt by addition of excess of triethylamine
7. customCrystals were then collected
8. customrecrystallized from hot water