HRID1640120

反应详情

EQUATION

反应方程式

HRID 1640120 的结构方程式

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

  1. temperatureThe reaction was heated
  2. temperatureat reflux for 18 h
  3. customThe solvent was evaporated
  4. dissolutionThe residue was redissolved in DCM
  5. additionsaturated NaHCO3 solution was added
  6. extractionThe mixture was extracted with DCM (2×)
  7. dry with materialthe combined organic solutions were dried over Na2SO4
  8. concentrationconcentrated