반응 #416585

ord-82d4d90b35544a80aca467bfe97325ee

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타To a 125 ml round-bottomed flask equipped with condenser and N2 inlet
  2. 2
    온도The reaction was heated
  3. 3
    온도at reflux for 5 days
  4. 4
    온도cooled
  5. 5
    여과the precipitate filtered
  6. 6
    세척washed with sodium bicarbonate
  7. 7
    건조dried over sodium sulfate
  8. 8
    workup.ADDITIONtreated with methylene chloride saturated with hydrochloride
  9. 9
    기타evaporated
  10. 10
    기타the residue triturated with ether
  11. 11
    기타to afford a white solid, m.p. 305°-307° C., 1.76 g (48%)

실험 절차

To a 125 ml round-bottomed flask equipped with condenser and N2 inlet were added 2.39 g (7.5 mmol) of 4-(4-(2-chloroethyl)phenyl)-2-methylthiazole hydrobromide, 1.59 g (7.5 mmol) of N-(1-naphthyl)piperazine, 1.31 ml (7.5 mmol) of diisopropylethylamine, 1.59 g (15 mmol) of sodium carbonate, 5 mg of sodium iodide, and 50 ml of methylisobutylketone. The reaction was heated at reflux for 5 days, cooled, and the precipitate filtered. The solid was taken up in methylene chloride, washed with sodium bicarbonate, dried over sodium sulfate, treated with methylene chloride saturated with hydrochloride, evaporated, and the residue triturated with ether to afford a white solid, m.p. 305°-307° C., 1.76 g (48%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04891375uspto-grants-1990_01