2-Chloro-4-(4-(3-(4-fluoro-3-methoxyphenyl)thioureido)-2-methyl-3-oxobutan-2-yl)benzenesulfonamide → HCID 178492991、化合物

HRID 1627359ノート

反応式

HRID 1627359 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([CH3:26])([C:10](=O)[CH2:11][NH:12][C:13]([NH:15][C:16]2[CH:21]=[CH:20][C:19]([F:22])=[C:18]([O:23][CH3:24])[CH:17]=2)=[S:14])[CH3:9])[CH:5]=[CH:4][C:3]=1[S:27]([NH2:30])(=[O:29])=[O:28]>CC(O)=O>[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([C:10]2[N:15]([C:16]3[CH:21]=[CH:20][C:19]([F:22])=[C:18]([O:23][CH3:24])[CH:17]=3)[C:13]([SH:14])=[N:12][CH:11]=2)([CH3:26])[CH3:9])[CH:5]=[CH:4][C:3]=1[S:27]([NH2:30])(=[O:29])=[O:28]

参加物

3

反応物 1

HCID 866622522-Chloro-4-(4-(3-(4-fluoro-3-methoxyphenyl)thioureido)-2-methyl-3-oxobutan-2-yl)benzenesulfonamide

生成物 1

HCID 178492991HCID 178492991、化合物収率 82.4%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 2-chloro-4-(4-(3-(4-fluoro-3-methoxyphenyl)thioureido)-2-methyl-3-oxobutan-2-yl)benzenesulfonamide (8.6 g, 18.1 mmol) in AcOH (100 mL) was refluxed 3 h. After the reaction was complete, the solution was cooled to room temperature and azeotroped with toluene. The residue was triturated with Et2O, filtered and dried to provide the title compound (6.8 g, 82% yield) as a light yellow solid. 1H NMR (400 MHz, CDCl3+MeOD) δ 7.92 (d, J=8.4 Hz, 1H), 7.09 (s, 1H), 7.06 (d, J=8.4 Hz, 1H), 6.97 (t, J=8.4 Hz, 1H), 6.89 (s, 1H), 6.38 (m, 1H), 6.13 (d, J=7.2 Hz, 1H), 3.58 (s, 3H), 1.54 (s, 6H); MS (EI) m/z 456 (MH+).

後処理

  1. customazeotroped with toluene
  2. customThe residue was triturated with Et2O
  3. filtrationfiltered
  4. customdried

出典と根拠

ORDレコード
ord-05aff3d08e264a2b93b7bf68043f802e
出典データセット
uspto-grants-2014_07
特許番号
US08785488B2

反応ノート

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