反応 #419856

ord-5cd8fdf9312248fd9d88485ade8b4112

反応方程式

COC(=O)c1ccc(Br)cc1
Methyl 4-bromobenzoate
O=C(c1ccccc1)c1cccc(O)c1
3-hydroxybenzophenone
O=C([O-])[O-].[K+].[K+]
potassium carbonate
COC(=O)c1ccc(COc2cccc(C(=O)c3ccccc3)c2)cc1
title compound
収率 99.0%
COC(=O)c1ccc(COc2cccc(C(=O)c3ccccc3)c2)cc1
Methyl 4-((3-benzoylphenoxy)methyl)benzoate
収率 99.0%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGto stir at room temperature for 16 hours
  2. 2
    抽出extracted with ethyl acetate
  3. 3
    抽出The organic extract
  4. 4
    洗浄was washed with brine
  5. 5
    乾燥dried (MgSO4)
  6. 6
    濃縮concentrated under reduced pressure
  7. 7
    その他The crude material was purified by silica gel chromatography
  8. 8
    洗浄eluting with 0-17% ethyl acetate in iso-hexane

実験手順

To a stirred solution of 3-hydroxybenzophenone (1.00 g, 5.04 mmol) in dimethyl formamide (10 mL), was added potassium carbonate (1.05 g, 7.61 mmol), and the mixture was stirred for 10 minutes at room temperature. Methyl 4-bromobenzoate (1.30 g, 6.05 mmol) in dimethyl formamide (5 mL) was added, and the reaction mixture allowed to stir at room temperature for 16 hours. The reaction mixture was diluted with water and extracted with ethyl acetate. The organic extract was washed with brine, dried (MgSO4), and concentrated under reduced pressure. The crude material was purified by silica gel chromatography eluting with 0-17% ethyl acetate in iso-hexane to afford the title compound (1.64 g, 99%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08877774B2uspto-grants-2014_11