반응 #1363

ord-fee902400dd24de2890c72bb0aeb17a9

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwere then added
  2. 2
    기타a reaction at 50° C. for 6 hours
  3. 3
    workup.DISTILLATIONAfter xylene was distilled off under reduced pressure, 300 ml of water
  4. 4
    workup.ADDITIONwere added
  5. 5
    workup.ADDITION10% sodium hydroxide was further added

실험 절차

A reactor was charged with 27 g (0.05 mole) of 11,15-dihydroxy-13-sulfoethyl-9,13,17-triazapentacosane and 100 g of xylene, to which 12 g (0.12 mole) of succinic anhydride were then added with stirring to conduct a reaction at 50° C. for 6 hours. After xylene was distilled off under reduced pressure, 300 ml of water were added, and 10% sodium hydroxide was further added to keep the pH of the reaction mixture at 7. Thereafter, the reaction mixture was subjected to electrodialysis and lyophilized, thereby obtaining 28 g (isolation yield: 76%) of 6,10-dihydroxy-4,12-dioctyl-3,13-dioxo-8-sulfoethyl-4,8,12-triaza-1,15-pentadecanedicarboxylic acid as white crystals.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05723655uspto-grants-1998_03