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Hydrochloric Acid → 1-[(3,4-Dichlorophenyl)methyl]-N-{4-[(2-hydroxyethyl)oxy]phenyl}-5-methyl-1H-1,2,3-triazole-4-carboxamide

HRID 450520
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HRID 450520 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH2:9][N:10]2[C:14]([CH3:15])=[C:13]([C:16]([NH:18][C:19]3[CH:24]=[CH:23][C:22]([O:25][CH2:26][CH2:27][O:28]C4CCCCO4)=[CH:21][CH:20]=3)=[O:17])[N:12]=[N:11]2)[CH:5]=[CH:6][C:7]=1[Cl:8].Cl>CO.C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH2:9][N:10]2[C:14]([CH3:15])=[C:13]([C:16]([NH:18][C:19]3[CH:20]=[CH:21][C:22]([O:25][CH2:26][CH2:27][OH:28])=[CH:23][CH:24]=3)=[O:17])[N:12]=[N:11]2)[CH:5]=[CH:6][C:7]=1[Cl:8]
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참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 595834191-[(3,4-Dichlorophenyl)methyl]-5-methyl-N-(4-{[2-(tetrahydro-2H-pyran-2-yloxy)ethyl]oxy}phenyl)-1H-1,2,3-triazole-4-carboxamide2회

생성물 1

HCID 426033611-[(3,4-Dichlorophenyl)methyl]-N-{4-[(2-hydroxyethyl)oxy]phenyl}-5-methyl-1H-1,2,3-triazole-4-carboxamide

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857
Ethyl Acetate
용매

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온도
60 °C

실험 절차

To a solution of the crude 1-[(3,4-dichlorophenyl)methyl]-5-methyl-N-(4-{[2-(tetrahydro-2H-pyran-2-yloxy)ethyl]oxy}phenyl)-1H-1,2,3-triazole-4-carboxamide (Intermediate 19) in methanol was added a saturated solution of HCl in ethyl acetate. The reaction was stirred to 60° C. for 18 hours. After evaporation, the title compound was obtained as a cream solid after recrystallisation from methanol (0.23 g, 54% from intermediate 6). HRMS calculated for C19H18Cl2N4O3 (M+H)+421.0834, found: 421.0837, Rt: 2.76 min. MP: 140° C.

후처리

  1. customAfter evaporation

출처 및 근거

ORD 기록
ord-de076dbf42d04e8ba425ad321f1b89ce
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08486977B2

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