反応 #170960

ord-babbe404bc1e4121af8d645fddc011eb

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度refluxed for 12 hours
  2. 2
    workup.DISTILLATIONAcetone was distilled off
  3. 3
    workup.ADDITIONwater (1500 ml) was added
  4. 4
    ろ過Crude 7 was filtered
  5. 5
    その他dried
  6. 6
    その他recrystallised from a mixture of ethyl acetate:hexane (1:5)

実験手順

To a mixture of 4-nitrophenol (100 g, 719 mmol) and anhydrous K2CO3 (400 gm, 2.894 mol) in anhydrous acetone (950 ml) was added methyl chloroacetate (114 g, 1.050 moles) and refluxed for 12 hours. Acetone was distilled off and water (1500 ml) was added. Crude 7 was filtered, dried and recrystallised from a mixture of ethyl acetate:hexane (1:5) to give pure 7 (110 g, 72.5%) as a white fluffy powder with an m.p between 97-98.4° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08846845B2uspto-grants-2014_09