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Acetonitrile → N-(4-((2-amino-3-chloropyridin-4-yl)oxy)-2-fluorophenyl)-1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxamide

HRID 870463
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인쇄 미리보기

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HRID 870463 반응식
[Cl:1][C:2]1[C:3](C(N)=O)=[N:4][CH:5]=[CH:6][C:7]=1[O:8][C:9]1[CH:14]=[CH:13][C:12]([NH:15][C:16]([C:18]2[C:19](=[O:31])[N:20]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[N:21]([CH3:24])[C:22]=2[CH3:23])=[O:17])=[C:11]([F:32])[CH:10]=1.C(OI(C1C=CC=CC=1)OC(=O)C)(=O)C.CC#[N:53]>CCOC(C)=O.O>[NH2:53][C:3]1[C:2]([Cl:1])=[C:7]([O:8][C:9]2[CH:14]=[CH:13][C:12]([NH:15][C:16]([C:18]3[C:19](=[O:31])[N:20]([C:25]4[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=4)[N:21]([CH3:24])[C:22]=3[CH3:23])=[O:17])=[C:11]([F:32])[CH:10]=2)[CH:6]=[CH:5][N:4]=1
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참가 물질

6

반응물 3

HCID 6342AcetonitrileHCID 76724Iodobenzene diacetateHCID 730510753-chloro-4-(4-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxamido)-3-fluorophenoxy)picolinamide

생성물 1

HCID 73053651N-(4-((2-amino-3-chloropyridin-4-yl)oxy)-2-fluorophenyl)-1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxamide수율 47%

시약·촉매·용매 2

HCID 962
Water
용매
HCID 8857Ethyl Acetate용매

반응 조건

온도
0 °C

실험 절차

A suspension of 3-chloro-4-(4-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxamido)-3-fluorophenoxy)picolinamide (379 mg, 0.764 mmol) in EtOAc (4.5 mL), CH3CN (4.5 mL) and H2O (2.5 mL) was cooled and stirred at 0° C. for 30 minutes, then PhI(OAc)2 (295 mg, 0.917 mmol) was added and the mixture was stirred for another 30 minutes at 0° C., then allowed to warmed up to rt and stirred for another 10 hours. Filtered and the filter cake was washed with EtOAc (5 mL). The filtrate was concentrated in vacuo and the residue was purified by a silica gel column chromatography (CH2Cl2/MeOH (v/v)=50/1) to give the title compound as a yellow solid (150 mg, 47.0%).

후처리

  1. temperaturewas cooled
  2. stirringthe mixture was stirred for another 30 minutes at 0° C.
  3. temperatureto warmed up to rt
  4. stirringstirred for another 10 hours
  5. filtrationFiltered
  6. washthe filter cake was washed with EtOAc (5 mL)
  7. concentrationThe filtrate was concentrated in vacuo
  8. customthe residue was purified by a silica gel column chromatography (CH2Cl2/MeOH (v/v)=50/1)

출처 및 근거

ORD 기록
ord-f5762c6ef80c45e78fbc2d436c77bf20
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08969388B1

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