HRID1166791

反应详情

EQUATION

反应方程式

HRID 1166791 的结构方程式

PROCEDURE

实验过程

To a suspension of 5-bromo-1-naphthylcarboxylic acid (5 g, 20 mmol) in 200 mL anhydrous MeOH was added 5 mL concentrated H2SO4 and refluxed overnight. The reaction was cooled to room temperature and concentrated to one-third the volume. The residue was diluted with water and extracted with diethyl ether. The organic layer was separated and washed with water (2×), dried over MgSO4, and concentrated. Silica gel column chromatography using hexane/ethyl acetate (2/11) gave 4.91 g (92%) of the product.

WORKUP

后处理

  1. temperaturerefluxed overnight
  2. concentrationconcentrated to one-third the volume
  3. additionThe residue was diluted with water
  4. extractionextracted with diethyl ether
  5. customThe organic layer was separated
  6. washwashed with water (2×)
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated