HRID11403

反应详情

EQUATION

反应方程式

HRID 11403 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a solution of 2-methylindole-4-acetic acid (53 g) in N,N-dimethylformamide (500 ml) was added dropwise allyl bromide (31 ml), and added anhydrous potassium carbonate (59 g). The mixture was stirred at 50° C. for 1 hour. After cooling to room temperature, the reaction mixture was poured into a mixture of 2N hydrochloric acid-ethyl acetate and then extracted with ethyl acetate. The extraction was washed with water and a saturated aqueous solution of sodium chloride, successively, dried and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (hexane-ethyl acetate) to give the title compound (43.5 g) having the following physical data.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. extractionextracted with ethyl acetate
  3. extractionThe extraction
  4. washwas washed with water
  5. dry with materiala saturated aqueous solution of sodium chloride, successively, dried
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by column chromatography on silica gel (hexane-ethyl acetate)