반응 #49651

ord-9964c7de6933407d9c2220728e01fc8c

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction mixture is refluxed for 10 hours under nitrogen
  2. 2
    온도after cooling it
  3. 3
    농축concentrated by evaporation under reduced pressure
  4. 4
    추출extracted with ether
  5. 5
    건조After drying with anhydrous sodium sulphate the organic phase
  6. 6
    농축is concentrated by evaporation
  7. 7
    workup.DISTILLATIONThe crude product is then distilled

실험 절차

3.4 g of sodium are dissolved in 120 ml of isopropanol and 11 g (0.067 mol) of 4-chloromethylpyridine-hydrochloride are added. The reaction mixture is refluxed for 10 hours under nitrogen, with stirring, then after cooling it is made weakly acidic with dilute hydrochloric acid and concentrated by evaporation under reduced pressure. The residue is made alkaline with 40% potassium carbonate solution and extracted with ether. After drying with anhydrous sodium sulphate the organic phase is concentrated by evaporation. The crude product is then distilled.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05422353uspto-grants-1995_06