反応 #1244247

ord-d5eca52ef81147d8b22377cb6ac8bcbf

反応方程式

CCC(=O)Cl
propanoyl chloride
Oc1ccc(N=Nc2ccccc2)cc1
4-Phenylazophenol
CCN(CC)CC
triethylamine
CCC(=O)Oc1ccc(N=Nc2ccccc2)cc1
product
収率 72.0%
CCC(=O)Oc1ccc(N=Nc2ccccc2)cc1
Propionic acid 4-phenylazo-phenyl ester
収率 72.0%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他reaction
  2. 2
    洗浄The reaction mixture was washed with water
  3. 3
    workup.ADDITIONdilute acid and brine
  4. 4
    乾燥dried with magnesium sulfate
  5. 5
    その他The solvent was evaporated

実験手順

4-Phenylazophenol (0.25 g, 1.26 mmoles) was dissolved in ether (5-10 mL) and triethylamine (0.26 mL) was added. Then propanoyl chloride (0.14 g 1.5 mmoles) in ether (1 mL) was added dropwise at room temperature. The mixture was stirred and reaction was rapidly completed. The reaction mixture was washed with water, dilute acid and brine and dried with magnesium sulfate. The solvent was evaporated to give 0.23 g (72%) of product. 1H NMR (CDCl3) δ=1.16 (3H, t, J=7.7), 2.40 (2H, q J=7.7), 7.25 (2H, m), 7.40-7.58 (3H, m), 7.88-8.0 (4H, m) ppm.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07807075B2uspto-grants-2010_10