HRID450039

反应详情

EQUATION

反应方程式

HRID 450039 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5-nitro-1H-indole (2.0 g, 12.3 mmol) in acetone (20 ml), powdered potassium hydroxide (3.4 g, 60.7 mmol, 5 eq) was added followed by the addition methyl iodide (2.61 g, 18.5 mmol, 1.5 eq) at 0° C. The reaction mixture was heated to reflux for 10 hr. The solvent was evaporated and water was added. The compound was extracted with ethyl acetate, dried over anhydrous sodium sulphate, filtered and the organic layer was concentrated to dryness to yield 1-methyl-5-nitro-1H-indole (2.0 g, 92%). The crude compound was used in the next stage without purification.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 10 hr
  3. customThe solvent was evaporated
  4. additionwater was added
  5. extractionThe compound was extracted with ethyl acetate
  6. dry with materialdried over anhydrous sodium sulphate
  7. filtrationfiltered
  8. concentrationthe organic layer was concentrated to dryness