Phenol → 2-Nitro-5-phenoxytoluene

HRID 862669

反応式

HRID 862669 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 27284182-Nitro-5-phenoxytoluene

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

反応条件

温度
20 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-defb0b4fd5514463b5bdb790daef7d08
出典データセット
uspto-grants-1998_02
特許番号
US05719164

関連ノート

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