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4-Fluorophenyl isocyanate → N-(4-Fluorophenyl)-4,4-dimethyl-1-(4-(trifluoromethyl)phenyl)-3,4-dihydro-isoquinoline-2(1H)-carboxamide

HRID 445287
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HRID 445287 반응식
[CH3:1][C:2]1([CH3:22])[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]([C:12]2[CH:17]=[CH:16][C:15]([C:18]([F:21])([F:20])[F:19])=[CH:14][CH:13]=2)[NH:4][CH2:3]1.[F:23][C:24]1[CH:29]=[CH:28][C:27]([N:30]=[C:31]=[O:32])=[CH:26][CH:25]=1>ClCCCl>[F:23][C:24]1[CH:29]=[CH:28][C:27]([NH:30][C:31]([N:4]2[CH2:3][C:2]([CH3:22])([CH3:1])[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[CH:5]2[C:12]2[CH:17]=[CH:16][C:15]([C:18]([F:21])([F:19])[F:20])=[CH:14][CH:13]=2)=[O:32])=[CH:26][CH:25]=1
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참가 물질

4

반응물 2

HCID 709554-Fluorophenyl isocyanateHCID 595363404,4-Dimethyl-1-(4-(trifluoromethyl)phenyl)-1,2,3,4-tetrahydroisoquinoline

생성물 1

HCID 59536389N-(4-Fluorophenyl)-4,4-dimethyl-1-(4-(trifluoromethyl)phenyl)-3,4-dihydro-isoquinoline-2(1H)-carboxamide

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

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온도
80 °C

실험 절차

A 25-mL round-bottomed flask was charged with 4,4-dimethyl-1-(4-(trifluoromethyl)phenyl)-1,2,3,4-tetrahydroisoquinoline (118 mg, 0.39 mmol), 4-fluorophenyl isocyanate (43.4 μL, 0.39 mmol) and DCE (5 mL). The reaction mixture was heated at 80° C. for 2 h and the solvent was then removed under vacuum. Purification by silica gel chromatography (20-30% EtOAc in hexanes) provided the title compound as a white solid. MS (ESI, positive ion) m/z: 443 (M+H).

후처리

  1. customthe solvent was then removed under vacuum
  2. customPurification by silica gel chromatography (20-30% EtOAc in hexanes)

출처 및 근거

ORD 기록
ord-03d4bbd4d6944d8f8089cb65b230b7b0
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08476297B2

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