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p-Fluoronitrobenzene → HCID 20187571、化合物

HRID 2308739
ノート
印刷プレビュー

反応式

HRID 2308739 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH:9]([OH:17])[CH:10]([F:16])[N:11]1[CH:15]=[N:14][CH:13]=[N:12]1.[OH-].[Na+].[N+:20]([C:23]1[CH:28]=[CH:27][C:26](F)=[CH:25][CH:24]=1)([O-:22])=[O:21]>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C(OCC)C>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH:9]([O:17][C:26]1[CH:27]=[CH:28][C:23]([N+:20]([O-:22])=[O:21])=[CH:24][CH:25]=1)[CH:10]([F:16])[N:11]1[CH:15]=[N:14][CH:13]=[N:12]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 9590p-FluoronitrobenzeneHCID 14798Sodium HydroxideHCID 20187544HCID 20187544、化合物

生成物 1

HCID 20187571HCID 20187571、化合物

試薬・触媒・溶媒 2

HCID 74236Tetrabutylammonium Bromide触媒HCID 3283Diethyl Ether溶媒

実験手順

With efficient stirring, 27.6 g of 1-(2,4-dichlorophenyl)-2-fluoro-2-(1H-1,2,4-triazolyl)ethanol (prepared in accordance with Example P1a) were added to a mixture of 250 ml of 2n NaOH solution, 250 ml of diethyl ether and 0.5 g of tetrabutylammonium bromide. 25 ml of 4-nitrofluorobenzene are added at 20° C. to this mixture, which is stirred for another 20 hours at room temperature. The separated ethereal phase is washed with water until neutral, dried over sodium sulfate, filtered and concentrated by evaporation. The crude oily product (35 g) is purified by chromatography through silica gel and melts after recrystallisation from diisopropyl ether/cyclohexanone at 98°-100° C.

後処理

  1. washThe separated ethereal phase is washed with water until neutral,
  2. dry with materialdried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated by evaporation
  5. customThe crude oily product (35 g) is purified by chromatography through silica gel and melts
  6. customafter recrystallisation from diisopropyl ether/cyclohexanone at 98°-100° C.

出典と根拠

ORDレコード
ord-72eb79977e9441e5ab2bfda5f824de94
出典データセット
uspto-grants-1987_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04690942

反応ノート

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