反应详情

A mixture of 1-cyano-4-hydroxy-7-phenoxy-isoquinoline-3-carboxylic acid methyl ester (82 mg, 0.26 mmol) and 3-amino-2,2-dimethyl-propionic acid (90 mg, 0.77 mmol) (ChemBridge) in 0.5 M NaOMe/MeOH (1.0 mL, 0.5 mmol) was microwaved at 120° C. for 40 min. Reaction mixture was concentrated and the residue was dissolved in water (70 mL). It was acidified by 1 N HCl to pH=3-4. Precipitate was collected, rinsed with water and dried. Crude product was triturated with MeOH (2 mL). solid was collected and dried to provide the title compound 54.4 mg (0.13 mmol) in 51% yield. LC-MS ESI−: 404.03 (M−1)−.

1. customwas microwaved at 120° C. for 40 min
2. customReaction mixture
3. concentrationwas concentrated
4. dissolutionthe residue was dissolved in water (70 mL)
5. customPrecipitate was collected
6. washrinsed with water
7. customdried
8. customCrude product was triturated with MeOH (2 mL)
9. customsolid was collected
10. customdried