反応 #1929022

ord-746948d6ac4a4c8eade3027451cd2569

反応方程式

O=C(Cl)c1ccccc1
Benzoyl chloride
O=[N+]([O-])c1cccc(O)c1
3-Nitrophenol
CCN(CC)CC
triethylamine
O
water
O=C(Oc1cccc([N+](=O)[O-])c1)c1ccccc1
3-nitrophenyl benzoate
収率 90.3%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGthe resulting solution was shaken at room temperature until full conversion
  2. 2
    乾燥The organic phase was dried over magnesium sulfate
  3. 3
    ろ過filtered
  4. 4
    その他the solvent was removed under reduced pressure

実験手順

3-Nitrophenol (1.716 g, 12.346 mmol) and triethylamine (1.6 mL, 12.346 mmol) were dissolved in 50 mL of dichloromethane. The solution was shaken 30 minutes at room temperature. Benzoyl chloride (1.43 mL, 12.346 mmol) was added drop by drop and the resulting solution was shaken at room temperature until full conversion as determined by thin-layer chromatography. Carbonated water (20 mL) was added three times. The organic phase was dried over magnesium sulfate, filtered and the solvent was removed under reduced pressure, thus affording 2.7080 g of a white solid corresponding to 3-nitrophenyl benzoate (11.144 mmol, yield=90%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08945522B2uspto-grants-2015_02