反应详情

温度

100 °C

To a solution of 0.075 g (0.17 mmol) of (+/−)-4-oxo-9-[(pyridine-2-carbonyl)-amino]-2-pyrimidin-4-yl-5,6,8,9-tetrahydro-4H-1,4a,7-triaza-benzocycloheptene-7-carboxylic acid ethyl ester (example 1) dissolved in 0.6 mL (3.44 mmol) of hydrobromic acid (33 wt % solution in glacial acetic acid). The resulting mixture was stirred at 100° C. for 8 hours, cooled and evaporated to dryness. Toluene was added to the residue and evaporated. MeOH added to the residue and evaporated. After an acido-basic work-up, the crude was triturated with diethyl ether and filtered to afford 0.035 g (45%) of the product as a white powder and free base.

1. temperaturecooled
2. customevaporated to dryness
3. additionToluene was added to the residue
4. customevaporated
5. additionMeOH added to the residue
6. customevaporated
7. customAfter an acido-basic work-up, the crude was triturated with diethyl ether
8. filtrationfiltered