Phenol → 2-Nitro-5-phenoxytoluene

HRID 1745

반응식

HRID 1745 반응식
[C:1]1([OH:7])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(=O)([O-])[O-].[K+].[K+].F[C:15]1[CH:16]=[CH:17][C:18]([N+:22]([O-:24])=[O:23])=[C:19]([CH3:21])[CH:20]=1>CN(C)C(=O)C>[N+:22]([C:18]1[CH:17]=[CH:16][C:15]([O:7][C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)=[CH:20][C:19]=1[CH3:21])([O-:24])=[O:23]

참가 물질

5

반응물 3

HCID 996PhenolHCID 11430Potassium CarbonateHCID 949565-Fluoro-2-nitrotoluene

생성물 1

HCID 27284182-Nitro-5-phenoxytoluene

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

반응 조건

온도
20 °C

실험 절차

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.

후처리

  1. stirringthe mixture was stirred at 70°-80° C. for 30 minutes
  2. temperaturethe mixture was heated at 135°-140° C. for 2 hours
  3. temperatureafter cooling
  4. concentrationconcentrated in vacuo
  5. additionthe residue was introduced into ice
  6. filtrationthe crystalline product was filtered off with suction
  7. washwashed with water
  8. customdried

출처 및 근거

ORD 기록
ord-7ccd2207c11e4dc982df4da8ca022082
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05726305

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