반응 #170960

ord-babbe404bc1e4121af8d645fddc011eb

반응 방정식

O=[N+]([O-])c1ccc(O)cc1
4-nitrophenol
O=C([O-])[O-].[K+].[K+]
K2CO3
COC(=O)CCl
methyl chloroacetate
COC(=O)COc1ccc([N+](=O)[O-])cc1
7
수율 72.5%
COC(=O)COc1ccc([N+](=O)[O-])cc1
Methyl (4-Nitro phenoxy)acetate
수율 72.5%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도refluxed for 12 hours
  2. 2
    workup.DISTILLATIONAcetone was distilled off
  3. 3
    workup.ADDITIONwater (1500 ml) was added
  4. 4
    여과Crude 7 was filtered
  5. 5
    기타dried
  6. 6
    기타recrystallised from a mixture of ethyl acetate:hexane (1:5)

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08846845B2uspto-grants-2014_09