HRID1604638

反应详情

EQUATION

反应方程式

HRID 1604638 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Sodium chloride (0.47 g) was added to a mixture of 4-tert-butyl-2-(5-formylbenzofuran-2-yl)thiazole (0.41 g), sodium hydrogenphosphate 12 water (0.23 g) and 2-methyl-2-butane (0.69 ml) in a mixed solvent of water (3 ml), tetrahydrofuran (7.5 ml) and tert-butanol (12.6 ml). After 4 hours, aqueous sodium hydrogensulfide solution was added to the mixture. The resulting mixture was extracted with ethyl acetate. The organic layer was washed with brine, dried over magnesium sulfate and concentrated under reduced pressure. The residue was dissolved in 1N-sodium hydroxide and the solution was treated with carbon powder and acidified with diluted hydrochloric acid. The resulting precipitates were collected and washed with water to give 2-(4-tert-butylthiazol-2-yl)benzofuran-5-carboxylic acid (0.38 g).

WORKUP

后处理

  1. extractionThe resulting mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. dissolutionThe residue was dissolved in 1N-sodium hydroxide
  6. additionthe solution was treated with carbon powder
  7. customThe resulting precipitates
  8. customwere collected
  9. washwashed with water