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

HRID 1433185
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HRID 1433185 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 178514703HCID 178514703, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-a7f2e45abf09461cafd7b3c2e4827c9d
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07612211B2

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