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Tributylphosphine → HCID 67528178, 화합물

HRID 2261853
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HRID 2261853 반응식
[CH3:1][O:2][C:3](=[O:20])[CH:4]=[CH:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]2[CH:17]=[CH:16][C:15]([OH:18])=[CH:14][C:13]=2[CH3:19])=[CH:8][CH:7]=1.[Cl:21][C:22]1[CH:27]=[CH:26][CH:25]=[C:24]([Cl:28])[C:23]=1[N:29]1[C:33]([CH2:34]O)=[C:32]([CH:36]([CH3:38])[CH3:37])[CH:31]=[N:30]1.N(C(N1CCCCC1)=O)=N[C:41](N1CCCCC1)=O.C(P(CCCC)CCCC)CCC>CCCCCC.C1(C)C=CC=CC=1>[CH2:1]([O:2][C:3](=[O:20])[CH:4]=[CH:5][C:6]1[CH:7]=[CH:8][C:9]([C:12]2[CH:17]=[CH:16][C:15]([O:18][CH2:34][C:33]3[N:29]([C:23]4[C:22]([Cl:21])=[CH:27][CH:26]=[CH:25][C:24]=4[Cl:28])[N:30]=[CH:31][C:32]=3[CH:36]([CH3:38])[CH3:37])=[CH:14][C:13]=2[CH3:19])=[CH:10][CH:11]=1)[CH3:41]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 13831TributylphosphineHCID 730421,1'-(Azodicarbonyl)dipiperidineHCID 57443256(1-(2,6-dichlorophenyl)-4-isopropyl-1H-pyrazol-5-yl)methanolHCID 67527577HCID 67527577, 화합물

생성물 1

HCID 67528178HCID 67528178, 화합물수율 85%

시약·촉매·용매 2

HCID 1140
Toluene
용매
HCID 8058Hexane용매

실험 절차

To a mixture of (108 mg, 0.403 mmol) 3-(4′-hydroxy-2′-methyl-biphenyl-4-yl)-acrylic acid methyl ester, [2-(2,6-dichloro-phenyl)-4-isopropyl-2H-pyrazol-3-yl]-methanol (126 mg, 0.443 mmol) and toluene (2.1 mL) is added 1,1′-(azodicarbonyl)dipiperidine (112 mg, 0.443 mmol) followed by tri-n-butylphosphine (109 μL, 0.443 mmol). The reaction is kept overnight at room temperature. The reaction mixture is diluted with hexane and the solid is filtered. The concentrated filtrate is purified via flash chromatography eluting with 15% ethyl acetate/heptane) to give 183 mg (85%) of the ester.

후처리

  1. filtrationthe solid is filtered
  2. customThe concentrated filtrate is purified via flash chromatography
  3. washeluting with 15% ethyl acetate/heptane)

출처 및 근거

ORD 기록
ord-9c0e120429ad48548bb2b277a339112d
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07846960B2

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