Acetic Anhydride → N-(4-Methoxy-2,3-dimethylphenyl)acetamide

HRID 1269818

反応式

HRID 1269818 の反応式
[CH3:1][C:2]1[C:7]([CH3:8])=[C:6]([N+:9]([O-])=O)[CH:5]=[CH:4][C:3]=1[O:12][CH3:13].[C:14](OC(=O)C)(=[O:16])[CH3:15].CCCCCC>CO.[Pd]>[CH3:13][O:12][C:3]1[CH:4]=[CH:5][C:6]([NH:9][C:14](=[O:16])[CH3:15])=[C:7]([CH3:8])[C:2]=1[CH3:1]

参加物

6

反応物 3

HCID 7918Acetic AnhydrideHCID 8058HexaneHCID 5964652,3-Dimethyl-4-nitroanisole

生成物 1

HCID 11275552N-(4-Methoxy-2,3-dimethylphenyl)acetamide収率 92%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

To a solution of 2,3-dimethyl-4-nitroanisole (1.04 g, 5.74 mmol) in methanol (20 ml) was added 10%-Pd/C (100 mg) at room temperature, and the resulting solution was stirred under a hydrogen atmosphere. After 1 hour, the reaction solution was filtered by the use of Celite and the filtrate was concentrated under reduced pressure and then dried. The residue was dissolved in ethyl acetate (10 ml), followed by adding thereto acetic anhydride (0.867 ml, 9.18 mmol), and the resulting mixture was refluxed. After 2 hours, hexane (70 ml) was poured into the reaction solution and the crystals formed were filtered under reduced pressure and then dried to obtain N-(4-methoxy-2,3-dimethylphenyl)acetamide (1.02 g, 92%).

後処理

  1. filtrationthe reaction solution was filtered by the use of Celite
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customdried
  4. dissolutionThe residue was dissolved in ethyl acetate (10 ml)
  5. additionby adding
  6. waitAfter 2 hours
  7. customthe crystals formed
  8. filtrationwere filtered under reduced pressure
  9. customdried

出典と根拠

ORDレコード
ord-1f386c4ce45247b7b06a434d5dcb06fa
出典データセット
uspto-grants-2007_04
特許番号
US07199147B2

関連ノート

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