反应 #6245

ord-65c49a041cb1404cbaeaf61fdae85da3

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.DISTILLATIONAfter the solvent was distilled off
  2. 2
    workup.ADDITIONbrine was added to the residue
  3. 3
    萃取The mixture was extracted with chloroform
  4. 4
    干燥dried over anhydrous magnesium sulfate
  5. 5
    workup.DISTILLATIONthe solvent was distilled off
  6. 6
    其他The residue was purified by column chromatography (eluent: ethanol/ethyl acetate=1:10)
  7. 7
    其他recrystallized from ethyl acetate

实验过程

Sodium borohydride [1.89 g (50 mmol)] was added to a solution of 2.82 g (10.0 mmol) of 4-(3-phthalimidopropyloxy)pyridine in 150 ml of ethanol. The mixture was stirred at room temperature for 15 minutes. After the solvent was distilled off, brine was added to the residue. The mixture was extracted with chloroform and dried over anhydrous magnesium sulfate, and then the solvent was distilled off. The residue was purified by column chromatography (eluent: ethanol/ethyl acetate=1:10), and then recrystallized from ethyl acetate to obtain 1.54 g of the desired compound (yield: 54.2%, colroless crystals).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05246948uspto-grants-1993_09