Hydroxyamine hydrochloride → N-hydroxy-1-(4-methyl-1,3-oxazol-5-yl)-1-phenylmethanimine

HRID 875188ノート

反応式

HRID 875188 の反応式
[CH3:1][C:2]1[N:3]=[CH:4][O:5][C:6]=1[C:7]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=O.Cl.[NH2:16][OH:17]>N1C=CC=CC=1>[OH:17][N:16]=[C:7]([C:6]1[O:5][CH:4]=[N:3][C:2]=1[CH3:1])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

参加物

4

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 53876795(4-Methyloxazol-5-yl)(phenyl)methanone

生成物 1

HCID 86650729N-hydroxy-1-(4-methyl-1,3-oxazol-5-yl)-1-phenylmethanimine収率 40.1%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
50 °C

実験手順

To a stirred solution of (4-methyl-1,3-oxazol-5-yl)(phenyl)methanone (1.34 g, 7.15 mmol) in pyridine (40 mL), was added hydroxylamine hydrochloride (1.24 g, 17.9 mmol) and the reaction mixture was heated at 50° C. for 15 h. The reaction mixture was concentrated in vacuo. Water (60 mL) was added and the mixture was extracted with ethyl acetate (3×30 ml). The combined organic phases were dried over MgSO4, filtered and concentrated in vacuo. Purification of the crude material on silica gel afforded N-hydroxy-1-(4-methyl-1,3-oxazol-5-yl)-1-phenylmethanimine (0.58 g, 39%).

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. additionWater (60 mL) was added
  3. extractionthe mixture was extracted with ethyl acetate (3×30 ml)
  4. dry with materialThe combined organic phases were dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customPurification of the crude material on silica gel

出典と根拠

ORDレコード
ord-04f2ffbe6de84699aa067f591767a2c3
出典データセット
uspto-grants-2015_03
特許番号
US08981111B2

反応ノート

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