HRID2240220

反应详情

EQUATION

反应方程式

HRID 2240220 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

477 mg (1.00 mmol) of 3-fluoro-4-[(1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-pyrrolo[2,3-b]pyridin-4-yl)methyl]aniline are dissolved in 4 ml of dichloromethane. 4.0 ml of trifluoroacetic acid are added, and the mixture is stirred at RT for 2 hours. The solution is concentrated to dryness. The residue is taken up in 15 ml of THF, and 15 ml of an aqueous 1 M lithium hydroxide solution are added. The solution is stirred at RT for 20 hours and then concentrated, and water is added. The mixture is extracted with ethyl acetate. The extract is dried over sodium sulfate and the solvent is removed under reduced pressure. The residue is purified by preparative HPLC.

WORKUP

后处理

  1. concentrationThe solution is concentrated to dryness
  2. addition15 ml of an aqueous 1 M lithium hydroxide solution are added
  3. stirringThe solution is stirred at RT for 20 hours
  4. concentrationconcentrated
  5. additionwater is added
  6. extractionThe mixture is extracted with ethyl acetate
  7. dry with materialThe extract is dried over sodium sulfate
  8. customthe solvent is removed under reduced pressure
  9. customThe residue is purified by preparative HPLC