반응 #8442

ord-32bf5b9791c7448ca1a7e797c6eb1088

반응 방정식

CC(=O)OC(C)=O
acetic anhydride
CCN(CC)CC
triethylamine
CN(C)c1ccccn1
dimethylaminopyridine
OCCOc1ccc(-c2nnnc(-c3cccc4ccccc34)c2-c2cccc3ccccc23)c(O)c1
product
OCCOc1ccc(-c2nnnc(-c3cccc4ccccc34)c2-c2cccc3ccccc23)c(O)c1
bis-α-naphthyl-(4-[2-hydroxy-ethoxy]-2-hydroxy-phenyl)-triazine
CC(=O)OCCOc1ccc(-c2nnnc(-c3cccc4ccccc34)c2-c2cccc3ccccc23)c(O)c1
bis-αnaphthyl-(4-[2-acetoxy-ethoxy]-2-hydroxy-phenyl)-triazine

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction mixture is heated to boiling
  2. 2
    기타the solvent is removed in vac
  3. 3
    세척The organic phase is washed with water
  4. 4
    건조dried with magnesium sulfate
  5. 5
    기타After removal of the solvent
  6. 6
    기타the residue is chromatographed on silica gel
  7. 7
    기타yielding the product

실험 절차

9.11 g of acetic anhydride, 18.1 g of triethylamine and 0.73 g of dimethylaminopyridine in 400 ml of anhydrous dichloromethane are added to the product from Example A9. The reaction mixture is heated to boiling. When the reaction is complete (monitoring by TLC), the solvent is removed in vac. and the residue is taken up in dichloromethane. The organic phase is washed with water and dried with magnesium sulfate. After removal of the solvent, the residue is chromatographed on silica gel, yielding the product having the following NMR data:

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07087753B2uspto-grants-2006_08