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Hydrochloric Acid → 2-[2-(4-Trifluoromethyl-phenoxymethyl)-1h-benzoimidazol-5-yl]-benzenesulfonamide hydrochloride salt

HRID 1433185
ノート
印刷プレビュー

反応式

HRID 1433185 の反応式
[F:1][C:2]([F:31])([F:30])[C:3]1[CH:29]=[CH:28][C:6]([O:7][CH2:8][C:9]2[NH:13][C:12]3[CH:14]=[CH:15][C:16]([C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=4[S:24]([NH2:27])(=[O:26])=[O:25])=[CH:17][C:11]=3[N:10]=2)=[CH:5][CH:4]=1.[ClH:32]>CCOC(C)=O>[ClH:32].[F:31][C:2]([F:1])([F:30])[C:3]1[CH:29]=[CH:28][C:6]([O:7][CH2:8][C:9]2[NH:13][C:12]3[CH:14]=[CH:15][C:16]([C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=4[S:24]([NH2:27])(=[O:26])=[O:25])=[CH:17][C:11]=3[N:10]=2)=[CH:5][CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 178514703HCID 178514703、化合物

生成物 1

HCID 1784795952-[2-(4-Trifluoromethyl-phenoxymethyl)-1h-benzoimidazol-5-yl]-benzenesulfonamide hydrochloride salt収率 77%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

2-[2-(4-trifluoromethyl-phenoxymethyl)-1H-benzoimidazol-5-yl]-benzenesulfonamide (19 g, 42.5 mmol) was dissolved in EtOAc (1000 mL) with warming to near boiling for complete dissolution. To the stirred solution at rt (orange in color) was added aqueous HCl (1 N, 850 mL, 20 eq.) all at once. The resulting suspension was stirred for 30 min at room temperature. The solid was filtered, washed with a small amount of EtOAc and water. The solid was dried in a high vacuum (2 torr) oven at 45° C. for 16 h, to provide (15.71 g) of the title compound in 77% yield. Calculated C21H16N3O3F3S×1.0 HCl×0.08H2O: C, 51.97; H, 3.56; N, 8.66; Cl 7.30; F 11.74; S 6.61; KF 0.30 Found: C, 52.11; H, 3.38; N, 8.37; Cl 7.43; F 11.53; S 6.56; KF 0.27

後処理

  1. temperaturewith warming
  2. dissolutionfor complete dissolution
  3. filtrationThe solid was filtered
  4. washwashed with a small amount of EtOAc and water
  5. customThe solid was dried in a high vacuum (2 torr) oven at 45° C. for 16 h

出典と根拠

ORDレコード
ord-a7f2e45abf09461cafd7b3c2e4827c9d
出典データセット
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07612211B2

反応ノート

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