HRID1481026
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
Methyl 4-(1-cyano-4-hydroxy-7-phenoxyisoquinoline-3-carboxamido)-4-methylpentanoate (16 mg, 0.04 mmol) was dissolved in MeOH (4 mL) and 2 N NaOH (4 mL). After stirring for 4 hours at room temperature, H2O (15 mL) and EtOAc (15 mL) were added. To the stirred mixture was added 1 N hydrochloric acid until pH was 1. The layers were separated and the aqueous layer was extracted twice with EtOAc. The combined organic layers were dried over MgSO4, concentrated, and purified by flash chromatography (0-30% MeOH/CH2Cl2 with 0.5% formic acid) to give the title compound in 14 mg. MS: (−) m/z 417.99 (M−1).
WORKUP
后处理
- customThe layers were separated
- extractionthe aqueous layer was extracted twice with EtOAc
- dry with materialThe combined organic layers were dried over MgSO4
- concentrationconcentrated
- custompurified by flash chromatography (0-30% MeOH/CH2Cl2 with 0.5% formic acid)