HRID342798
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
To a stirred solution of 5-bromo-1-(4-nitro-benzyl)-1H-indole-2-carboxylic acid ethyl ester (2.3 g, 5.7 mmol) in ethanol/water (2:1, 45 ml) at room temperature was added potassium hydroxide (0.96 g, 17.1 mmol). The solution was warmed to reflux for about 3 hours, cooled, and most of the ethanol was removed under reduced pressure. To the residue was added water, 0.5N sodium hydroxide and methylene chloride, and the two-phase mixture was suction filtered to remove some insoluble material. The aqueous layer was acidified to pH 2 with 6N hydrochloric acid, and the precipitate was filtered off, washed with water, and air dried to afford the title compound, (1.66 g).
WORKUP
后处理
- temperatureThe solution was warmed
- temperatureto reflux for about 3 hours
- temperaturecooled
- custommost of the ethanol was removed under reduced pressure
- additionTo the residue was added water, 0.5N sodium hydroxide and methylene chloride
- filtrationfiltered
- customto remove some insoluble material
- filtrationthe precipitate was filtered off
- washwashed with water, and air
- customdried