HRID2392286

反应详情

EQUATION

反应方程式

HRID 2392286 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of methyl 5-chloro-4-(1-methyl-1H-1,2,3-triazol-5-yl)-2-thiophenecarboxylate (400 mg, 1.55 mmol) and 1N LiOH (2.0 ml, 2.0 mmol) in THF (6 ml) was stirred at rt overnight. After removal of THF, the residue was diluted with 10 ml of H2O and washed with DCM (10 ml×2). The aqueous layer was acidified to pH 3 with 1N HCl and then extracted with EtOAc (30 ml×4). The organic layers were combined and concentrated to give 370 mg of the title compound as a white solid. LCMS (ES) m/z 244.0 (M+H)+

WORKUP

后处理

  1. customAfter removal of THF
  2. additionthe residue was diluted with 10 ml of H2O
  3. washwashed with DCM (10 ml×2)
  4. extractionextracted with EtOAc (30 ml×4)
  5. concentrationconcentrated