HRID2264611

反应详情

EQUATION

反应方程式

HRID 2264611 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

8.9 ml LiOH (1 M in H2O) are added to a solution of 2.80 g (5.9 mMol) 6-[1-(3-trifluoromethyl-phenylcarbamoyl)-2,3-dihydro-1H-indol-5-yloxy]-pyrimidine-4-carboxylic acid ethyl ester in 20 ml THF. After 1 h at rt, the mixture is concentrated under reduced pressure, the residue re-dissolved in EtOAc and 1 M HCl, the aqueous layer separeted off and extracted twice with EtOAc. The organic phases are washed twice with 1 M HCl, water and brine, dried (Na2SO4) and concentrated to the title compound: MS: [M−1]=443; HPLC: AtRet=12.9.

WORKUP

后处理

  1. concentrationthe mixture is concentrated under reduced pressure
  2. dissolutionthe residue re-dissolved in EtOAc
  3. extractionextracted twice with EtOAc
  4. washThe organic phases are washed twice with 1 M HCl, water and brine
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated to the title compound