反応 #8442

ord-32bf5b9791c7448ca1a7e797c6eb1088

反応方程式

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

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction mixture is heated to boiling
  2. 2
    その他the solvent is removed in vac
  3. 3
    洗浄The organic phase is washed with water
  4. 4
    乾燥dried with magnesium sulfate
  5. 5
    その他After removal of the solvent
  6. 6
    その他the residue is chromatographed on silica gel
  7. 7
    その他yielding the product

実験手順

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:

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07087753B2uspto-grants-2006_08