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N-(2-benzoyl-4-chlorophenyl)-methyl-hydrazinecarbothioamide → 7-Chloro-3-methyl-5-phenyl-2-thioxo-1,2-dihydro-3H-1,3,4-benzotriazepine

HRID 26642
ノート
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反応式

HRID 26642 の反応式
[C:1]([C:9]1[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:10]=1[NH:16][C:17]([N:19]([CH3:21])[NH2:20])=[S:18])(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>C(O)CC>[Cl:15][C:13]1[CH:12]=[CH:11][C:10]2[NH:16][C:17](=[S:18])[N:19]([CH3:21])[N:20]=[C:1]([C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[C:9]=2[CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 13972523N-(2-benzoyl-4-chlorophenyl)-methyl-hydrazinecarbothioamide

生成物 1

HCID 1355779247-Chloro-3-methyl-5-phenyl-2-thioxo-1,2-dihydro-3H-1,3,4-benzotriazepine

試薬・触媒・溶媒 1

HCID 10311-Propanol溶媒

実験手順

A mixture containing 20.0 grams of N-(2-benzoyl-4-chlorophenyl)-methyl-hydrazine-carbothioamide (Example 2) in 250 ml of n-propanol was refluxed for about 2 hours. The yellow precipitate was cooled in an ice bath, and the resulting yellow precipitate was collected, washed with isopropanol and air dried to yield 7-chloro-1,3-dihydro-3-methyl-5-phenyl-2H-1,3,4-benzotriazepine-2-thione as a yellow solid. Additional product was obtained upon evaporation of the solvent under vacuum. The melting point was found to be 188°-190° C.

後処理

  • temperaturewas refluxed for about 2 hours
  • temperatureThe yellow precipitate was cooled in an ice bath
  • customthe resulting yellow precipitate was collected
  • washwashed with isopropanol and air
  • customdried
  • 出典と根拠

    ORDレコード
    ord-d21c709304e94413bd8d318d2e975eed
    出典データセット
    uspto-grants-1979_04
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US04151166

    反応ノート

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