3,4-Dimethoxybenzonitrile → 3,4-Dimethoxythiobenzamide

HRID 1421944

反応式

HRID 1421944 の反応式
[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]

参加物

4

反応物 2

HCID 748423,4-DimethoxybenzonitrileHCID 2723949Thioacetamide

生成物 1

HCID 27584903,4-Dimethoxythiobenzamide収率 61.9%

試薬・触媒・溶媒 1

HCID 10920465N,N-dimethylformamide;hydrochloride溶媒

反応条件

温度
90 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-faf2b22a52924dcca2aa946d5eed631b
出典データセット
uspto-grants-2000_06
特許番号
US06080764

関連ノート

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