HRID1481070
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 1-cyano-4-hydroxy-7-phenoxy-isoquinoline-3-carboxylic acid methyl ester (140 mg, 0.44 mmol), 2 M NaOH (3 mL), MeOH (3 mL) and THF (3 mL) was stirred for 5 h at r.t. The resulting mixture was concentrated to approximately one-third of its original volume and then placed in an ice bath. Hydrochloric acid (1 M) was added until pH ˜2, and the mixture was extracted with EtOAc. The organic layer was dried over MgSO4 and concentrated to give 132 mg of the title compound as a white solid. MS: (−) m/z 305.26 (M−1).
WORKUP
后处理
- concentrationThe resulting mixture was concentrated to approximately one-third of its original volume
- customplaced in an ice bath
- additionHydrochloric acid (1 M) was added until pH ˜2
- extractionthe mixture was extracted with EtOAc
- dry with materialThe organic layer was dried over MgSO4
- concentrationconcentrated