반응 #156179

ord-114ce8ebf149461e96c1a1b402fcc09f

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출followed by extraction
  2. 2
    세척The organic layer was washed with water
  3. 3
    건조saturated saline, and dried with anhydrous sodium sulfate
  4. 4
    기타After condensation under reduced pressure
  5. 5
    기타the residue was purified by silica gel column chromatography (ethyl acetate:methanol=20:1→4:1)
  6. 6
    기타condensed under reduced pressure

실험 절차

(2-Pyridin-3-yl-ethyl)-pyridin-4-ylmethyl-amine (210 mg) and N-ethyldiisopropylamine (0.34 ml) were added to a DMF solution (2 ml) of 1-chloro-3-iodopropane (0.16 ml). The mixture was stirred at room temperature overnight. Water was added to the reaction mixture, followed by extraction using ethyl acetate. The organic layer was washed with water and then saturated saline, and dried with anhydrous sodium sulfate. After condensation under reduced pressure, the residue was purified by silica gel column chromatography (ethyl acetate:methanol=20:1→4:1). The purified product was condensed under reduced pressure to give the title compound (74 mg) as a colorless oily matter.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08822453B2uspto-grants-2014_09