Acetic Anhydride → 2-(4-fluorophenyl)-5-methyl-2H-1,2,3-triazol-4-yl acetate

HRID 623694ノート

反応式

HRID 623694 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[N:12]=[C:11]([CH3:13])[CH:10]=[N+:9]2[O-])=[CH:4][CH:3]=1.[C:15]([O:18]C(=O)C)(=[O:17])[CH3:16]>>[C:15]([O:18][C:10]1[C:11]([CH3:13])=[N:12][N:8]([C:5]2[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=2)[N:9]=1)(=[O:17])[CH3:16]

参加物

3

反応物 2

HCID 7918Acetic AnhydrideHCID 901115092-(4-fluorophenyl)-4-methyl-2H-1,2,3-triazole 1-oxide2 回

生成物 1

HCID 901095002-(4-fluorophenyl)-5-methyl-2H-1,2,3-triazol-4-yl acetate

実験手順

2-(4-Fluorophenyl)-4-methyl-2H-1,2,3-triazole 1-oxide (i.e. the product of Step A, 6.6 g, 34 mmol) was added to acetic anhydride (47 mL, 500 mmol), and the reaction mixture was stirred at reflux for 28 h. The reaction was concentrated under reduced pressure. The residue was taken up in ethyl acetate, washed successively with water and saturated aqueous sodium chloride solution, dried with magnesium sulfate and concentrated under reduced pressure to afford the title compound (7.8 g) as a beige solid. The title compound was used directly in the next step without further purification.

後処理

  1. temperatureat reflux for 28 h
  2. concentrationThe reaction was concentrated under reduced pressure
  3. washwashed successively with water and saturated aqueous sodium chloride solution
  4. dry with materialdried with magnesium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-b48e8abb97ed4654b32961d88556da64
出典データセット
uspto-grants-2016_04
特許番号
US09302999B2

反応ノート

読み込み中…