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Water → 3,5-Bis-(2-trifluoromethylpyridin-4-yloxy)benzonitrile

HRID 353205
ノート
印刷プレビュー

反応式

HRID 353205 の反応式
F[C:2]1[CH:3]=[C:4]([CH:7]=[C:8](F)[CH:9]=1)[C:5]#[N:6].[C:11](=[O:14])([O-])[O-].[K+].[K+].[F:17][C:18]([F:27])([F:26])[C:19]1[CH:24]=[C:23]([OH:25])[CH:22]=[CH:21][N:20]=1.O>CN(C)C(=O)C.C(OCC)(=O)C.CCCCCCC>[F:27][C:18]([F:17])([F:26])[C:19]1[CH:24]=[C:23]([O:25][C:2]2[CH:3]=[C:4]([CH:7]=[C:8]([O:14][C:11]3[CH:22]=[CH:21][N:20]=[C:19]([C:18]([F:27])([F:26])[F:17])[CH:24]=3)[CH:9]=2)[C:5]#[N:6])[CH:22]=[CH:21][N:20]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 5872043,5-DifluorobenzonitrileHCID 178516505HCID 178516505、化合物

生成物 1

HCID 115609193,5-Bis-(2-trifluoromethylpyridin-4-yloxy)benzonitrile

試薬・触媒・溶媒 2

HCID 31374Dimethylacetamide溶媒
HCID 21899848
Ethylacetate heptane
溶媒

反応条件

温度
150 °C

実験手順

Under an atmosphere of nitrogen, 0.556 g (4.0 mmol) of 3,5-difluorobenzonitrile was initially charged in 10 ml of N,N-dimethylacetamide, and 1.22 g (8.8 mmol) of potassium carbonate were added a little at a time at room temperature. 1.305 g (8.00 mmol) of 2-(trifluoromethyl)pyridin-4-ol were then added and the mixture was heated at 150° C. for 30 h and cooled to room temperature, water and ethyl acetate/heptane (1:1) were added to the reaction solution and the solution was stirred for a number of minutes. The phases were separated and the organic phase was washed repeatedly with water and finally with saturated sodium chloride solution and then dried over sodium sulfate, filtered and concentrated. HPLC of the crude product gave 3,5-bis-(2-trifluoromethylpyridin-4-yloxy)benzonitrile in the form of white crystals.

後処理

  1. temperaturecooled to room temperature
  2. customThe phases were separated
  3. washthe organic phase was washed repeatedly with water and finally with saturated sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-8bd2a47560894c11a47af83b98b5e951
出典データセット
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06750222B2

反応ノート

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