HRID323405

反应详情

EQUATION

反应方程式

HRID 323405 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Combine 5-formylsalicylic acid (5.0 g, 30.1 mmol), potassium carbonate (16.6 g, 120.4 mmol), and methyl iodide (34.06 g, 240 mmol) in acetone (20 mL). Heat to reflux. After 12 hours, cool and extract five times with ethyl acetate. Combine the organic layers and extract with brine. Dry over MgSO4, filter, and concentrate in vacuo to give a residue. Chromatograph the residue on silica gel eluting with ethyl acetate/hexane 1/1 to give methyl 2-methoxy-5-formylbenzoate: Rf=0.44 (silica gel, 1/1 ethyl acetate/hexane).

WORKUP

后处理

  1. temperatureHeat to reflux
  2. temperaturecool
  3. extractionextract five times with ethyl acetate
  4. extractionextract with brine
  5. dry with materialDry over MgSO4
  6. filtrationfilter
  7. concentrationconcentrate in vacuo
  8. customto give a residue