Water → 4'-Dimethylaminoacetanilide

HRID 2093040

反応式

HRID 2093040 の反応式
[CH3:1][N:2]([CH3:10])[C:3]1[CH:8]=[CH:7][C:6]([NH2:9])=[CH:5][CH:4]=1.C(N(CC)CC)C.[C:18](OC(=O)C)(=[O:20])[CH3:19].O>ClCCl>[CH3:1][N:2]([CH3:10])[C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:18](=[O:20])[CH3:19])=[CH:5][CH:4]=1

参加物

6

反応物 4

HCID 962WaterHCID 7472N,N-dimethyl-p-phenylenediamineHCID 7918Acetic AnhydrideHCID 8471Triethylamine

生成物 1

HCID 819684'-Dimethylaminoacetanilide収率 69%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of N,N-dimethylbenzene-1,4-diamine (1.0 eq) in dichloromethane, triethylamine (2.2 eq) was added at 0° C. and stirred for 15 min. To the above mixture was then added a solution of acetic anhydride (1.0 eq) in dichloromethane at 0° C., after addition the reaction was continued at room temperature for 5 hrs. Water was added and the organic layer was separated, dried over anhydrous Na2SO4, concentrated under reduced pressure to afford crude product, which, on purification by column chromatography afforded the desired N-[4-(dimethylamino)phenyl]acetamide. (Yield=69%)

後処理

  1. additionafter addition the reaction
  2. waitwas continued at room temperature for 5 hrs
  3. customthe organic layer was separated
  4. dry with materialdried over anhydrous Na2SO4
  5. concentrationconcentrated under reduced pressure
  6. customto afford crude product, which
  7. customon purification by column chromatography

出典と根拠

ORDレコード
ord-caed95fe1a9247fd8670bf899b7624dc
出典データセット
uspto-grants-2013_05
特許番号
US08440830B2

関連ノート

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