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p-Fluoronitrobenzene → HCID 20187571, 화합물

HRID 2308739
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HRID 2308739 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 9590p-FluoronitrobenzeneHCID 14798Sodium HydroxideHCID 20187544HCID 20187544, 화합물

생성물 1

HCID 20187571HCID 20187571, 화합물

시약·촉매·용매 2

HCID 74236Tetrabutylammonium Bromide촉매HCID 3283Diethyl Ether용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-72eb79977e9441e5ab2bfda5f824de94
출처 데이터셋
uspto-grants-1987_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04690942

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