1-Fluoro-4-(1-isothiocyanatoethyl)benzene → HCID 10094291、化合物

HRID 1352515ノート

反応式

HRID 1352515 の反応式
[CH2:1]([C:8]1[C:9]([C:13]2[CH:18]=[CH:17][C:16]([NH2:19])=[CH:15][CH:14]=2)=[N:10][O:11][CH:12]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[F:20][C:21]1[CH:31]=[CH:30][C:24]([CH:25]([N:27]=[C:28]=[S:29])[CH3:26])=[CH:23][CH:22]=1>CN(C)C=O>[CH2:1]([C:8]1[C:9]([C:13]2[CH:14]=[CH:15][C:16]([NH:19][C:28]([NH:27][CH:25]([C:24]3[CH:23]=[CH:22][C:21]([F:20])=[CH:31][CH:30]=3)[CH3:26])=[S:29])=[CH:17][CH:18]=2)=[N:10][O:11][CH:12]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 5195361-Fluoro-4-(1-isothiocyanatoethyl)benzeneHCID 21100737HCID 21100737、化合物

生成物 1

HCID 10094291HCID 10094291、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 4-(4-benzyl-isoxazol-3-yl)-phenylamine and 4-fluoro-α-methyl-benzyl isothiocyanate in dimethylformamide (5 mL) is stirred for 12 hours at room temperature. The reaction mixture is then partitioned between ethyl acetate and water. The organic layer is washed with saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give 1.4 g crude product as a yellow solid. The latter is recrystallized from ethyl acetate/hexane to give 0.9 g product as a yellow solid. MS: m/z 433 (M+H)+.

後処理

  1. customThe reaction mixture is then partitioned between ethyl acetate and water
  2. washThe organic layer is washed with saturated aqueous sodium chloride
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto give 1.4 g crude product as a yellow solid
  6. customThe latter is recrystallized from ethyl acetate/hexane

出典と根拠

ORDレコード
ord-1776ada67fe54e45ae9af346f1806bc4
出典データセット
uspto-grants-2007_05
特許番号
US07220768B2

反応ノート

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