反应详情

A mixture of 3-[(1-cyano-7-cyclohexyloxy-4-hydroxy-isoquinoline-3-carbonyl)-amino]-2,2-dimethyl-propionic acid tert-butyl ester (55 mg, 0.118 mmol) in (½) TFA/CH2Cl2 (3 mL) was stirred at room temperature for 3 h and concentrated. Residue was taken up with 30 mL of water and the resultant suspension was basified by 1 N NaOH to pH=9-10. The clear solution was then acidified by 1 N HCl to pH=3-4. Precipitate was collected and dried. Crude product was triturated with MeOH (3 mL). Solid was collected and dried in vacuo to provide the title compound 8.6 mg (0.02 mmol) in 18% yield. LC-MS ESI−: 410.00 (M−1)−.

1. concentrationconcentrated
2. customPrecipitate was collected
3. customdried
4. customCrude product was triturated with MeOH (3 mL)
5. customSolid was collected
6. customdried in vacuo