O-Methylhydroxylamine → Phenyl(4-(trifluoromethyl)phenyl)methanone O-methyl oxime

HRID 1622569

反応式

HRID 1622569 の反応式
[C:1]1([C:7]([C:9]2[CH:14]=[CH:13][C:12]([C:15]([F:18])([F:17])[F:16])=[CH:11][CH:10]=2)=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:19][O:20][NH2:21].CCOC(C)=O>N1C=CC=CC=1>[CH3:19][O:20][N:21]=[C:7]([C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)[C:9]1[CH:14]=[CH:13][C:12]([C:15]([F:18])([F:17])[F:16])=[CH:11][CH:10]=1

参加物

5

反応物 3

HCID 4113O-Methylhydroxylamine2 回HCID 8857Ethyl AcetateHCID 697674-(Trifluoromethyl)benzophenone

生成物 1

HCID 76047680Phenyl(4-(trifluoromethyl)phenyl)methanone O-methyl oxime収率 99.4%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a 100-mL round-bottomed flask, phenyl(4-(trifluoromethyl)phenyl)-methanone (1.0105 g, 4.039 mmol) and methoxyamine (0.4208 g, 5.038 mmol) were dissolved in pyridine (10 mL). The mixture was stirred at rt overnight. Additional methoxyamine (0.1625 g) was added, and the solution was stirred at rt for 7 h. EtOAc was added and the organic phase was washed with water, 1 N HCl (2×), water, and then with brine. The organic phase was dried over sodium sulfate, filtered and concentrated in vacuo to afford a clear oil. The oil thus obtained was purified by Biotage (EtOAc/hexanes 0-20%) to afford the title compound (1.12 g, 99.4%) as a clear oil.

後処理

  1. stirringthe solution was stirred at rt for 7 h
  2. washthe organic phase was washed with water, 1 N HCl (2×), water
  3. dry with materialThe organic phase was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customto afford a clear oil
  7. customThe oil thus obtained
  8. customwas purified by Biotage (EtOAc/hexanes 0-20%)

出典と根拠

ORDレコード
ord-329d0f7369864518b4df91bcd748e839
出典データセット
uspto-grants-2014_07
特許番号
US08778941B2

関連ノート

読み込み中…