반응 #1364

ord-edde2bbf24c7456a8918ccba8422abf0

반응 방정식

CCCCCCCCNCC(O)CN(CCS(=O)(=O)O)CC(O)CNCCCCCCCC
11,15-dihydroxy-13-sulfoethyl-9,13,17-triazapentacosane
O=C1C=CC(=O)O1
maleic anhydride
CCCCCCCCN(CC(O)CN(CCS(=O)(=O)O)CC(O)CN(CCCCCCCC)C(=O)C=CC(=O)O)C(=O)C=CC(=O)O
6,10-dihydroxy-4,12-dioctyl-3,13-dioxo-8-sulfoethyl-4,8,12-triaza-1,14-pentadecadiene-1,15-dicarboxylic acid
수율 80.0%

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 20 g (0.04 mole) of 11,15-dihydroxy-13-sulfoethyl-9,13,17-triazapentacosane and 100 g of xylene, to which 10 g (0.1 mole) of maleic 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 22 g (isolation yield: 80%) of 6,10-dihydroxy-4,12-dioctyl-3,13-dioxo-8-sulfoethyl-4,8,12-triaza-1,14-pentadecadiene-1,15-dicarboxylic acid as white powder.

출처

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