HRID2249665

反应详情

EQUATION

反应方程式

HRID 2249665 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

In 100 ml of N,N-dimethylformamide are dissolved 10.0 g of methyl salicylate, 18.1 g of potassium carbonate and 11.3 ml of isobutyl iodide. The solution is heated under reflux for 1.5 hours with stirring. The reaction mixture is added to a mixture of ethyl acetate and water, pH is adjusted to 2.0 with 6 mol/L hydrochloric acid, and the organic layer is separated. The organic layer thus obtained is washed with water and saturated aqueous solution of sodium chloride successively and dried over anhydrous magnesium sulfate, and then the solvent is distilled off under reduced pressure. The residue thus obtained is purified by silica gel column chromatography (eluent; n-hexane:ethyl acetate=95:5) to obtain 4.2 g of methyl 2-isobutoxybenzoate as a light yellow oily product.

WORKUP

后处理

  1. temperatureThe solution is heated
  2. temperatureunder reflux for 1.5 hours
  3. customthe organic layer is separated
  4. customThe organic layer thus obtained
  5. washis washed with water and saturated aqueous solution of sodium chloride successively
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationthe solvent is distilled off under reduced pressure
  8. customThe residue thus obtained
  9. customis purified by silica gel column chromatography (eluent; n-hexane:ethyl acetate=95:5)