HRID1466824

反应详情

EQUATION

反应方程式

HRID 1466824 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

3-(6-Chloro-1-isothiazol-4-yl-2-methyl-1H-indol-3-ylsulfanyl)-benzoic acid ethyl ester (0.073 g, 0.182 mmol) was dissolved in THF (2 mL), H2O (0.75 mL) and MeOH (0.75 mL) and LiOH.H2O (0.040 g, 0.953 mmol) was added. The reaction was stirred at room temperature and monitored by analytical LCMS. When no starting material remained the reaction was diluted with H2O and EtOAc and citric acid was added until pH 3 was reached. The layers were separated and the aqueous layer was extracted with EtOAc. The combined organic portions were washed with H2O, dried over MgSO4 and concentrated. The residue was purified via silica gel chromatography (0-5% MeOH in DCM) to give the title compound.

WORKUP

后处理

  1. additionwas added until pH 3
  2. customThe layers were separated
  3. extractionthe aqueous layer was extracted with EtOAc
  4. washThe combined organic portions were washed with H2O
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated
  7. customThe residue was purified via silica gel chromatography (0-5% MeOH in DCM)