3-Iodophenylisothiocyanate → HCID 57773569、化合物

HRID 333128ノート

反応式

HRID 333128 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[S:21])[NH:10][C:11]2[CH:16]=[CH:15][C:14]([S:17]([NH2:20])(=[O:19])=[O:18])=[CH:13][CH:12]=2)=[CH:4][CH:3]=1.[I:22][C:23]1[CH:28]=[CH:27][CH:26]=[C:25]([N:29]=[C:30]=[S:31])[CH:24]=1>C(#N)C>[I:22][C:23]1[CH:24]=[C:25]([NH:29][C:30](=[S:31])[NH:1][C:2]2[CH:3]=[CH:4][C:5]([NH:8][C:9](=[S:21])[NH:10][C:11]3[CH:16]=[CH:15][C:14]([S:17]([NH2:20])(=[O:18])=[O:19])=[CH:13][CH:12]=3)=[CH:6][CH:7]=2)[CH:26]=[CH:27][CH:28]=1

参加物

4

反応物 2

HCID 1510833-IodophenylisothiocyanateHCID 577735954-(3-(4-Aminophenyl)thioureido)benzenesulfonamide

生成物 1

HCID 57773569HCID 57773569、化合物収率 78%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of 4-(3-(4-aminophenyl)thioureido)benzenesulfonamide (0.322 g, 1.0 mmol) in acetonitrile was added 1-iodo-3-isothiocyanatobenzene (0.261 g, 1.0 mmol). The mixture was stirred at room temperature overnight. The solvent was evaporated under reduced pressure and water was added into the crude reaction mixture. The precipitate which formed was filtered, and dried to afford the title product as a white solid (0.452 g, 78%). 1H NMR (400 MHz, DMSO) δ 10.05 (s, 1H), 10.02 (s, 1H), 9.90 (s, 1H), 9.81 (s, 1H), 7.94 (t, J=1.8 Hz, 1H), 7.74 (d, J=8.8 Hz, 2H), 7.68 (d, J=8.8 Hz, 2H), 7.48-7.41 (m, 5H), 7.12 (t, J=8.0 Hz, 1H); MS (ESI), 584 (M+H)+.

後処理

  1. customThe solvent was evaporated under reduced pressure and water
  2. additionwas added into the crude
  3. customreaction mixture
  4. customThe precipitate which formed
  5. filtrationwas filtered
  6. customdried

出典と根拠

ORDレコード
ord-e30dc672821d47d0b44b8dfd786187ae
出典データセット
uspto-grants-2014_11
特許番号
US08877970B2

反応ノート

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