反应 #2045020

ord-979c1d994dc040a9be53471a14f4c4a7

反应方程式

O=[N+]([O-])c1ccc(O)cc1
4-Nitro phenol
O=C([O-])[O-].[K+].[K+]
K2CO3
COC(=O)CCl
methyl chloroacetate
COC(=O)COc1ccc([N+](=O)[O-])cc1
31
收率 72.5%
COC(=O)COc1ccc([N+](=O)[O-])cc1
Methyl(4-Nitro phenoxy)acetate
收率 72.5%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度refluxed for 12 hours
  2. 2
    workup.DISTILLATIONAcetone was distilled off
  3. 3
    workup.ADDITIONwater (1500 ml) added
  4. 4
    过滤Crude 31 was filtered
  5. 5
    其他dried
  6. 6
    其他recrystallised from a mixture of ethyl acetate:hexane (1:5)

实验过程

To a mixture of 4-Nitro phenol (100 g, 719 mmol) and anhydrous K2CO3 (400 g, 2.894 moles) 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) added. Crude 31 was filtered, dried and recrystallised from a mixture of ethyl acetate:hexane (1:5) to give pure 31 (110 g, 72.5%) as a white fluffy powder. M.p: 97-98.4° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08409559B2uspto-grants-2013_04