Toluene → 96605-61-7

HRID 1018878

反応式

HRID 1018878 の反応式
[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([NH:10][C:11]([CH3:13])=[O:12])[CH:5]=1)=[O:3].CO[CH:16](OC)[N:17]([CH3:19])[CH3:18].C1(C)C=CC=CC=1>CCOC(C)=O>[CH3:16][N:17]([CH3:19])[CH:18]=[CH:1][C:2]([C:4]1[CH:5]=[C:6]([NH:10][C:11](=[O:12])[CH3:13])[CH:7]=[CH:8][CH:9]=1)=[O:3]

参加物

5

反応物 3

HCID 1140TolueneHCID 78373Dimethylformamide dimethyl acetalHCID 3462023'-Acetamidoacetophenone

生成物 1

HCID 5341241596605-61-7収率 95%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 3-acetamidoacetophenone (3 kg; Lancaster), dimethylformamide dimethylacetal (7 L; Lancaster) and toluene (12 L; Mallinckrodt) is heated at reflux and methanol collected as it is formed. The mixture is heated overnight and a precipitate forms during this time. The reaction may be monitored by TLC analysis (EtOAc: starting material Rf=0.46; product Rf=0.10) to ensure it goes to completion. The reaction mixture is cooled and the solid is collected by filtration. The cake is washed with hexanes (4 L) then dried to give 3.77 kg (95% yield) of a light yellow powder.

後処理

  1. temperatureis heated
  2. temperatureat reflux
  3. custommethanol collected as it
  4. customis formed
  5. temperatureThe mixture is heated overnight
  6. customThe reaction
  7. temperatureThe reaction mixture is cooled
  8. filtrationthe solid is collected by filtration
  9. washThe cake is washed with hexanes (4 L)
  10. customthen dried

出典と根拠

ORDレコード
ord-48a1dc3095074abcb50d8b845d4c0c4a
出典データセット
uspto-grants-2002_11
特許番号
US06485746B1

関連ノート

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