HRID1869257

反应详情

EQUATION

反应方程式

HRID 1869257 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5-fluoro-3-methyl-1H-indole-2-carboxylic acid (8.49 g, 43.9 mmol) and copper metal (0.35 g, 5.5 mmol) in distilled quinoline (22 mL) was heated to reflux for 3 hours. The copper powder was filtered off and the filtrate was brought to pH 3 at 0° C. with a 6N aqueous solution of hydrochloric acid. The solution was extracted with ether (200 mL) and the organics washed with saturated sodium chloride (200 mL), dried over magnesium sulfate and concentrated in vacuo to give 5-fluoro-3-methyl-1H-indole as a brown solid. MS (ES) m/z 150.0.

WORKUP

后处理

  1. temperatureto reflux for 3 hours
  2. filtrationThe copper powder was filtered off
  3. customwas brought to pH 3 at 0° C. with a 6N aqueous solution of hydrochloric acid
  4. extractionThe solution was extracted with ether (200 mL)
  5. washthe organics washed with saturated sodium chloride (200 mL)
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated in vacuo