反应详情

A mixture of 4-hydroxy-1-methyl-7-phenoxy-isoquinoline-3-carboxylic acid methyl ester (120 mg, 0.39 mmol) and beta-alanine (242 mg, 2.72 mmol) in 0.5 M NaOMe/MeOH solution (4.5 mL, 2.25 mmol) was microwaved at 120° C. for 30 min. Reaction mixture was concentrated and dissolved in water (100 mL). It was acidified by 1 N HCl to pH=3-4. Gummy precipitate was collected by filtration and dissolved in EtOAc. It was dried over MgSO4, filtered and concentrated to provide the title compound 116 mg (0.32 mmol) in 81% yield. LC-MS ESI−: 365.16 (M−1)−.

1. customwas microwaved at 120° C. for 30 min
2. customReaction mixture
3. concentrationwas concentrated
4. dissolutiondissolved in water (100 mL)
5. filtrationGummy precipitate was collected by filtration
6. dissolutiondissolved in EtOAc
7. dry with materialIt was dried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated