HRID2219449
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureto reflux for 3 hours
- filtrationThe copper powder was filtered off
- customwas brought to pH 3 at 0° C. with a 6N aqueous solution of hydrochloric acid
- extractionThe solution was extracted with ether (200 mL)
- washthe organics washed with saturated sodium chloride (200 mL)
- dry with materialdried over magnesium sulfate
- concentrationconcentrated in vacuo