HRID1028020
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 88 °C
PROCEDURE
实验过程
A mixture of methyl 6-bromo-1-cyclopentyl-5-fluoro-1H-indole-3-carboxylate (3.4 g, 10 mmol), dimethylzinc (1.2 M, 16.7 mL, 20 mmol) and PdCl2dppf (163 mg, 0.2 mmol) in dioxane (20 mL) was stirred at 88° C. for 2 hr under nitrogen atmosphere. The mixture was then cooled and methanol was added in slowly followed by 2 N HCl. The mixture was treated with ethyl acetate, washed with water and brine, dried and evaporated. The residue was purified by flash chromatography with dichloromethane and hexane (1:1) to give methyl 1-cyclopentyl-5-fluoro-6-methyl-1H-indole-3-carboxylate (2.66 g, yield 97%).
WORKUP
后处理
- temperatureThe mixture was then cooled
- washwashed with water and brine
- customdried
- customevaporated
- customThe residue was purified by flash chromatography with dichloromethane and hexane (1:1)