反应详情

A mixture of 1-cyano-4-hydroxy-7-phenoxy-isoquinoline-3-carboxylic acid methyl ester (88 mg, 0.27 mmol) and beta-alanine (122 mg, 1.38 mmol) in 2.2 ml of 0.5 M NaOMe/MeOH solution was microwaved at 120° C. for 10 min. Reaction mixture was concentrated. The residue was dissolved in water (80 ml) and extracted with EtOAc, which was discarded. The aqueous layer was acidified by 1 N HCl to pH=3-4 and extracted with EtOAc. Organic layer was dried over MgSO4, filtered and concentrated. The crude product was triturated with hot MeOH and then CH2Cl2. Solid was collected and dried to provide the title compound 24 mg (0.064 mmol) in 24% yield.

1. customwas microwaved at 120° C. for 10 min
2. customReaction mixture
3. concentrationwas concentrated
4. dissolutionThe residue was dissolved in water (80 ml)
5. extractionextracted with EtOAc, which
6. extractionextracted with EtOAc
7. dry with materialOrganic layer was dried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated
10. customThe crude product was triturated with hot MeOH
11. customSolid was collected
12. customdried