Toluene → 96605-61-7

HRID 1018878

반응식

HRID 1018878 반응식
[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]

참가 물질

5

반응물 3

HCID 1140TolueneHCID 78373Dimethylformamide dimethyl acetalHCID 3462023'-Acetamidoacetophenone

생성물 1

HCID 5341241596605-61-7수율 95%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-48a1dc3095074abcb50d8b845d4c0c4a
출처 데이터셋
uspto-grants-2002_11
특허 번호
US06485746B1

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