HRID1807713

反应详情

EQUATION

反应方程式

HRID 1807713 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

tert-Butyl 4-(4-aminobenzoyl)piperazine-1-carboxylate (4.98 mmol, 1.520 g) was dissolved in dichloromethane and trifluoroacetic acid added. The reaction was left overnight and then treated to SCX purification. The intermediate amine was combined with 2-(4-(bromomethyl)phenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol (4.98 mmol, 1.678 g) and potassium carbonate (4.98 mmol, 0.688 g) in acetonitrile (30 mL) and stirred overnight. The reaction was concentrated under reduced pressure and the residue partitioned between water and ethyl acetate. The organic layer was separated and concentrated under reduced pressure. Purification by SCX column chromatography and silica chromatography (eluting with ethyl acetate) gave the title compound (1.25 g).

WORKUP

后处理

  1. additiontreated to SCX purification
  2. concentrationThe reaction was concentrated under reduced pressure
  3. customthe residue partitioned between water and ethyl acetate
  4. customThe organic layer was separated
  5. concentrationconcentrated under reduced pressure
  6. customPurification
  7. washby SCX column chromatography and silica chromatography (eluting with ethyl acetate)