반응 #7294

ord-40c021b30b0b44aeab08b6c10bded196

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과the formed precipitate of S-dibenzylcysteamine was collected by filtration
  2. 2
    추출The product was extracted with ether (3×100 mL)
  3. 3
    세척the organic phase was successively washed with brine (2×100 mL)
  4. 4
    건조dried over MgSO4
  5. 5
    기타the solvent evaporated in vacuo
  6. 6
    기타It could, however be recrystallized from ethyl acetate

실험 절차

To a suspension of 0.1 mole cysteamine hydrochloride in 20 mL methanol were added 13.6 mL of 25% ammonia solution, followed by dropwise addition of 0.12 mole benzyl bromide at room temperature. The mixture was stirred for 0.5 h, and the formed precipitate of S-dibenzylcysteamine was collected by filtration. The product was extracted with ether (3×100 mL) and the organic phase was successively washed with brine (2×100 mL), dried over MgSO4 and the solvent evaporated in vacuo. The crude product was essentially pure enough for the next step. It could, however be recrystallized from ethyl acetate. Yield 86%, of white solid. m.p. 85–6° C. NMR (CDCl3) in agreement with the title compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07084244B2uspto-grants-2006_08