HRID515318

反应详情

EQUATION

反应方程式

HRID 515318 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-(Piperidin-4-ylthio)aniline (6.69 mmol, 1.3946 g), 2-(4-(bromomethyl)phenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol (6.69 mmol, 2.256 g), and potassium carbonate (13.39 mmol, 1.850 g) were combined in acetonitrile (20 mL) and the reaction mixture stirred at room temperature for 1 hour. The reaction mixture was concentrated under vacuum, and partitioned between dichloromethane and water. The organic layer was separated, dried, and concentrated under vacuum. The residue was purified by silica column chromatography (eluting with 2.5-5% methanol/dichloromethane gradient) to afford the title compound (1.93 g). MS m/z 465.0 [M+H]+

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under vacuum
  2. custompartitioned between dichloromethane and water
  3. customThe organic layer was separated
  4. customdried
  5. concentrationconcentrated under vacuum
  6. customThe residue was purified by silica column chromatography (eluting with 2.5-5% methanol/dichloromethane gradient)