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

HRID 1918196노트

반응식

HRID 1918196 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 before leaving the medium to stir at ambient temperature for 3 h. The ethanol is subsequently evaporated 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 and then the aqueous phase is extracted 5 times with 150 ml of ethyl acetate. The organic phases are subsequently combined, dried over sodium sulphate and concentrated under vacuum. 7.82 g of compound are obtained.

후처리

  1. custombefore leaving the medium
  2. customThe ethanol is subsequently evaporated under vacuum
  3. customthe residue obtained
  4. customThe organic phase is separated
  5. extractionthe aqueous phase is extracted 5 times with 150 ml of ethyl acetate
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-b5c03cbfe0924a4b927ab6cab3a33257
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08618301B2

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