HRID342798

反应详情

EQUATION

反应方程式

HRID 342798 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe solution was warmed
  2. temperatureto reflux for about 3 hours
  3. temperaturecooled
  4. custommost of the ethanol was removed under reduced pressure
  5. additionTo the residue was added water, 0.5N sodium hydroxide and methylene chloride
  6. filtrationfiltered
  7. customto remove some insoluble material
  8. filtrationthe precipitate was filtered off
  9. washwashed with water, and air
  10. customdried