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Tributylphosphine → Methyl(4-fluoro-6-((1-methyl-3-(trifluoromethyl)-1H-pyrazol-5-yl)methoxy)-1-benzothiophen-3-yl)acetate

HRID 591563
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HRID 591563 반응식
C(P(CCCC)CCCC)CCC.[CH3:14][N:15]1[C:19]([CH2:20][OH:21])=[CH:18][C:17]([C:22]([F:25])([F:24])[F:23])=[N:16]1.[CH3:26][O:27][C:28](=[O:41])[CH2:29][C:30]1[C:34]2[C:35]([F:40])=[CH:36][C:37](O)=[CH:38][C:33]=2[S:32][CH:31]=1.C1CCN(C(N=NC(N2CCCCC2)=O)=O)CC1>C1COCC1>[CH3:26][O:27][C:28](=[O:41])[CH2:29][C:30]1[C:34]2[C:35]([F:40])=[CH:36][C:37]([O:21][CH2:20][C:19]3[N:15]([CH3:14])[N:16]=[C:17]([C:22]([F:23])([F:24])[F:25])[CH:18]=3)=[CH:38][C:33]=2[S:32][CH:31]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 13831TributylphosphineHCID 730421,1'-(Azodicarbonyl)dipiperidineHCID 58456726(1-Methyl-3-(trifluoromethyl)-1H-pyrazol-5-yl)methanolHCID 129359611Methyl(4-fluoro-6-hydroxy-1-benzothiophen-3-yl)acetate

생성물 1

HCID 118667066Methyl(4-fluoro-6-((1-methyl-3-(trifluoromethyl)-1H-pyrazol-5-yl)methoxy)-1-benzothiophen-3-yl)acetate수율 74.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a mixture of tri-n-butylphosphine (0.793 mL), (1-methyl-3-(trifluoromethyl)-1H-pyrazol-5-yl)methanol (187 mg), methyl(4-fluoro-6-hydroxy-1-benzothiophen-3-yl)acetate (250 mg) and THF (dry) (15 mL) was added ADDP (801 mg) at room temperature. The mixture was stirred at room temperature for 2 h and then concentrated in vacuo. To the residue was added IPE and the insoluble materials were removed by filtration. The filtrate was concentrated in vacuo. The residue was purified by silica gel column chromatography (NH, EtOAc/hexane) and silica gel column chrothatography (EtOAc/hexane) to give the title compound (310 mg). The crystals were recrystallized from acetone-hexane.

후처리

  1. concentrationconcentrated in vacuo
  2. additionTo the residue was added IPE
  3. customthe insoluble materials were removed by filtration
  4. concentrationThe filtrate was concentrated in vacuo
  5. customThe residue was purified by silica gel column chromatography (NH, EtOAc/hexane) and silica gel column chrothatography (EtOAc/hexane)

출처 및 근거

ORD 기록
ord-f73cf3400212418c9d87da9c4c09feab
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09238639B2

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