3,4-Dimethoxybenzonitrile → 3,4-Dimethoxythiobenzamide

HRID 1421944

반응식

HRID 1421944 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[C:6]#[N:7].C(N)(=[S:15])C>Cl.CN(C=O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[C:6]([NH2:7])=[S:15]

참가 물질

4

반응물 2

HCID 748423,4-DimethoxybenzonitrileHCID 2723949Thioacetamide

생성물 1

HCID 27584903,4-Dimethoxythiobenzamide수율 61.9%

시약·촉매·용매 1

HCID 10920465N,N-dimethylformamide;hydrochloride용매

반응 조건

온도
90 °C

실험 절차

25 g of 3,4-dimethoxybenzonitrile and 23 g of thioacetamide were dissolved in 120 ml of 10% hydrochloric acid-DMF. The solution was heated at 90° C. for 3 hours. The solution was further heated at 130° C. for 5 hours to conduct a reaction. The solvent was removed by distillation. The residue was washed twice with 100 ml of diethyl ether. Similar washing was conducted with 100 ml of water. The resulting crystals were collected by filtration and dried. Recrystallization from methanol was conducted to obtain 18.7 g of 3,4-dimethoxythiobenzamide as light brown columnar crystals.

후처리

  1. temperatureThe solution was further heated at 130° C. for 5 hours
  2. customa reaction
  3. customThe solvent was removed by distillation
  4. washThe residue was washed twice with 100 ml of diethyl ether
  5. washSimilar washing
  6. filtrationThe resulting crystals were collected by filtration
  7. customdried
  8. customRecrystallization from methanol

출처 및 근거

ORD 기록
ord-faf2b22a52924dcca2aa946d5eed631b
출처 데이터셋
uspto-grants-2000_06
특허 번호
US06080764

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