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

HRID 1918196ノート

反応式

HRID 1918196 の反応式
[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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b5c03cbfe0924a4b927ab6cab3a33257
出典データセット
uspto-grants-2013_12
特許番号
US08618301B2

反応ノート

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