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Hydrochloric Acid → 3-{3-[(2-Chloro-3-trifluoromethyl-benzyl)-2,2-diphenylethylamino]-propoxy}-phenylamine

HRID 902632
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HRID 902632 반응식
C(OC(=O)[NH:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([O:14][CH2:15][CH2:16][CH2:17][N:18]([CH2:33][C:34]2[CH:39]=[CH:38][CH:37]=[C:36]([C:40]([F:43])([F:42])[F:41])[C:35]=2[Cl:44])[CH2:19][CH:20]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH:9]=1)(C)(C)C.Cl>O1CCOCC1>[Cl:44][C:35]1[C:36]([C:40]([F:41])([F:42])[F:43])=[CH:37][CH:38]=[CH:39][C:34]=1[CH2:33][N:18]([CH2:19][CH:20]([C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1)[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)[CH2:17][CH2:16][CH2:15][O:14][C:10]1[CH:9]=[C:8]([NH2:7])[CH:13]=[CH:12][CH:11]=1
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 10175511(3-{3-[(2-Chloro-3-trifluoromethyl-benzyl)-diphenylethyl-amino]-propoxy}-phenyl)-carbamic acid tert-butyl ester

생성물 1

HCID 101287483-{3-[(2-Chloro-3-trifluoromethyl-benzyl)-2,2-diphenylethylamino]-propoxy}-phenylamine수율 96.1%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

To N-(3-{3-[(2-Chloro-3-trifluoromethyl-benzyl)-2,2-diphenylethyl-amino]-propoxy}-phenyl)-carbamic acid tert-butyl ester (492 mg, 0.77 mmol) dissolved in dioxane (5 mL) was added a 4.0 M solution of HCl in dioxane (5 mL). The solution was maintained for 20 hours after which the solvent was removed under reduced pressure. The residue was dissolved in dichloromethane and washed twice with saturated NaHCO3, dried over Na2SO4, and concentrated to give 0.4 g (0.74 mmol, 96%) of the title compound as a yellow oil. MS (ESI) 539.2

후처리

  1. temperatureThe solution was maintained for 20 hours after which the solvent
  2. customwas removed under reduced pressure
  3. dissolutionThe residue was dissolved in dichloromethane
  4. washwashed twice with saturated NaHCO3
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-517b823aa52946ef8ca86369b66d95bb
출처 데이터셋
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07365085B2

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