Ethanol → 2-(4-bromopyridin-2-yl)-1-(4-fluorophenyl)ethanone Oxime

HRID 1190857노트

반응식

HRID 1190857 반응식
[Br:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([CH2:8][C:9]([C:11]2[CH:16]=[CH:15][C:14]([F:17])=[CH:13][CH:12]=2)=O)[CH:3]=1.C(O)C.N1C=CC=CC=1.Cl.[NH2:28][OH:29]>O.C(OCC)(=O)C>[Br:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([CH2:8][C:9]([C:11]2[CH:16]=[CH:15][C:14]([F:17])=[CH:13][CH:12]=2)=[N:28][OH:29])[CH:3]=1

참가 물질

7

반응물 4

HCID 702EthanolHCID 1049PyridineHCID 443297Hydroxyamine hydrochlorideHCID 672466172-(4-Bromopyridin-2-yl)-1-(4-fluorophenyl)ethanone

생성물 1

HCID 866713742-(4-bromopyridin-2-yl)-1-(4-fluorophenyl)ethanone Oxime수율 104.3%

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

7.5 g (24.26 mmol) of 2-(4-bromopyridin-2-yl)-1-(4-fluorophenyl)ethanone are placed in a round-bottomed flask containing 100 mL of absolute ethanol. 20 mL (247.78 mmol) of pyridine and 7.08 g (101.88 mmol) of hydroxylamine monohydrochloride are added, and the medium is then stirred for 3 hours at room temperature. The ethanol is then evaporated off under vacuum and the residue obtained is taken up in 250 mL of water and 250 mL of ethyl acetate. The organic phase is separated out and the aqueous phase is then extracted 5 times with 150 mL of ethyl acetate. The organic phases are then combined, dried over sodium sulfate and concentrated under vacuum. 7.82 g of compound are obtained.

후처리

  1. customThe ethanol is then evaporated off under vacuum
  2. customthe residue obtained
  3. customThe organic phase is separated out
  4. extractionthe aqueous phase is then extracted 5 times with 150 mL of ethyl acetate
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-a19f904a0d514eb9b75f3363a468b31c
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08680096B2

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