Acetic Anhydride → N-(2-Fluorophenyl)acetamide

HRID 408118

反応式

HRID 408118 の反応式
C(O[C:5](=[O:7])[CH3:6])(=O)C.[F:8][C:9]1[CH:15]=[CH:14][CH:13]=[CH:12][C:10]=1[NH2:11]>O>[C:5]([NH:11][C:10]1[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=1[F:8])(=[O:7])[CH3:6]

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 95842-Fluoroaniline

生成物 1

HCID 67860N-(2-Fluorophenyl)acetamide収率 88%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

Acetic anhydride (57 mL, 0.6 mol) was added slowly, over approximately 40 min, to stirred 2-fluoroaniline (27, 55.7 g, 0.5 mol) under cooling (water bath) to maintain the reaction temperature at 60° C. to 70° C. After 10 hours more, the reaction mixture was poured into H2O, the whole was extracted with ethyl acetate (2×300 mL). The combined organic extracts were washed with 5% aqueous NaHCO3, brine, dried (K2CO3), filtered and concentrated to provide the title compound as a white solid (67.0 g, 88%).

後処理

  1. temperatureto maintain the reaction temperature at 60° C. to 70° C
  2. extractionthe whole was extracted with ethyl acetate (2×300 mL)
  3. washThe combined organic extracts were washed with 5% aqueous NaHCO3, brine
  4. dry with materialdried (K2CO3)
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-a5aa74e6c47942a594e2d3676c1b0851
出典データセット
uspto-grants-2014_06
特許番号
US08759336B2

関連ノート

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