تفاعل #1841

ord-7ccd2207c11e4dc982df4da8ca022082

معادلة التفاعل

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

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
20°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGthe mixture was stirred at 70°-80° C. for 30 minutes
  2. 2
    درجة الحرارةthe mixture was heated at 135°-140° C. for 2 hours
  3. 3
    درجة الحرارةafter cooling
  4. 4
    تركيزconcentrated in vacuo
  5. 5
    workup.ADDITIONthe residue was introduced into ice
  6. 6
    ترشيحthe crystalline product was filtered off with suction
  7. 7
    غسيلwashed with water
  8. 8
    أخرىdried

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05726305uspto-grants-1998_03