HRID1640120
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
To a solution of 6-hydroxy-1,2,3,4-tetrahydroisoquinoline-3-carboxylic acid (1.0 g, 5.2 mmol) in MeOH (50 mL) was added thionyl chloride (0.56 mL, 7.8 mmol) slowly. The reaction was heated at reflux for 18 h and then cooled to rt. The solvent was evaporated. The residue was redissolved in DCM and saturated NaHCO3 solution was added. The mixture was extracted with DCM (2×) and the combined organic solutions were dried over Na2SO4 and concentrated to give methyl 6-hydroxyisoquinoline-3-carboxylate as a white solid (0.72 g, 67%). LCMS: (FA) ES+ 208.2.
WORKUP
后处理
- temperatureThe reaction was heated
- temperatureat reflux for 18 h
- customThe solvent was evaporated
- dissolutionThe residue was redissolved in DCM
- additionsaturated NaHCO3 solution was added
- extractionThe mixture was extracted with DCM (2×)
- dry with materialthe combined organic solutions were dried over Na2SO4
- concentrationconcentrated