反应详情

温度

90 °C

To a solution of 0.075 g (0.22 mmol) of (+/−)-9-ethyl-4-oxo-2-pyrimidin-4-yl-5,6,8,9-tetrahydro-4H-1,4-a,7-triaza-benzocycloheptene-7-carboxylic acid ethyl ester (example 10) dissolved in 0.8 mL of glacial acetic acid was added 0.77 mL (4.37 mmol) of hydrobromic acid (33 wt % solution in glacial acetic acid). The resulting mixture was stirred at 90° C. for 4 hours, cooled and evaporated to dryness. Methanol was added to the residue and evaporated. Toluene was added to the residue and evaporated. The crude was triturated with diethyl ether and filtered to afford 0.068 g of the product as a white powder (88%).

1. temperaturecooled
2. customevaporated to dryness
3. additionMethanol was added to the residue
4. customevaporated
5. additionToluene was added to the residue
6. customevaporated
7. customThe crude was triturated with diethyl ether
8. filtrationfiltered