反应 #1841

ord-7ccd2207c11e4dc982df4da8ca022082

反应方程式

Oc1ccccc1
phenol
O=C([O-])[O-].[K+].[K+]
potassium carbonate
Cc1cc(F)ccc1[N+](=O)[O-]
5-fluoro-2-nitrotoluene
Cc1cc(Oc2ccccc2)ccc1[N+](=O)[O-]
2-Nitro-5-phenoxytoluene

反应条件

温度
20°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGthe mixture was stirred at 70°-80° C. for 30 minutes
  2. 2
    温度the mixture was heated at 135°-140° C. for 2 hours
  3. 3
    温度after cooling
  4. 4
    浓缩concentrated in vacuo
  5. 5
    workup.ADDITIONthe residue was introduced into ice
  6. 6
    过滤the crystalline product was filtered off with suction
  7. 7
    洗涤washed with water
  8. 8
    其他dried

实验过程

14.1 g (150 mmol) of phenol were dissolved in 120 ml of anhydrous N,N-dimethylacetamide, while stirring, 20.6 g (150 mmol) of finely powdered potassium carbonate were added and the mixture was stirred at 70°-80° C. for 30 minutes. After cooling to 20° C., 23.25 g (18.3 ml, 150 mmol) of 5-fluoro-2-nitrotoluene were added dropwise, the mixture was heated at 135°-140° C. for 2 hours and, after cooling, concentrated in vacuo, the residue was introduced into ice and the crystalline product was filtered off with suction, washed with water and dried, 30 g, melting point 43°-46° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05726305uspto-grants-1998_03