반응 #951139

ord-7480bf7e66ae44a6a213c452bc87cad5

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwas added
  2. 2
    세척The reaction mixture was washed with a 1N aqueous solution of sodium hydroxide and water
  3. 3
    기타dried
  4. 4
    workup.DISTILLATIONThen the solvent was distilled off
  5. 5
    기타The residue was purified by column chromatography (eluent: ethyl acetate)

실험 절차

In 100 ml of methylene chloride were dissolved 11.1 g (100 mmol) of 4-mercaptopyridine and 13.9 ml (100 mmol) of triethylamine, and 9.04 ml (100 mmol) of 3-bromo-1-propanol was added. The mixture was stirred at room temperature for hours. The reaction mixture was washed with a 1N aqueous solution of sodium hydroxide and water and dried. Then the solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate) to obtain 14.2 g of the desired compound (yield: 83.9%, yellow oil).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05561147uspto-grants-1996_10