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Sodium Acetate → HCID 68782696, 화합물

HRID 2266452
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HRID 2266452 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5](OS(C(F)(F)F)(=O)=O)=[C:6]2[C:11]=1[N:10]=[C:9]([CH3:12])[C:8]([S:13][C:14]1[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=1)=[C:7]2[CH3:21].C([Si]([O:37][C:38]([O:40][CH3:41])=[CH2:39])(C)C)(C)(C)C.C([O-])(=O)C.[Na+]>CN(C)C=O.C(OCC)(=O)C.[Pd].C(=CC(C=CC1C=CC=CC=1)=O)C1C=CC=CC=1.C(=CC(C=CC1C=CC=CC=1)=O)C1C=CC=CC=1.C1(P(C2C=CC=CC=2)[C-]2C=CC=C2)C=CC=CC=1.[C-]1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=C1.[Fe+2]>[CH3:41][O:40][C:38](=[O:37])[CH2:39][C:5]1[CH:4]=[CH:3][C:2]([Cl:1])=[C:11]2[C:6]=1[C:7]([CH3:21])=[C:8]([S:13][C:14]1[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=1)[C:9]([CH3:12])=[N:10]2
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참가 물질

8

반응물 3

HCID 517045Sodium AcetateHCID 45644911-(tert-Butyldimethylsilyloxy)-1-methoxyetheneHCID 86631433HCID 86631433, 화합물

생성물 1

HCID 68782696HCID 68782696, 화합물

시약·촉매·용매 4

HCID 1542701,5-Diphenylpenta-1,4-dien-3-one;palladium촉매
HCID 635956
Ferrocene-1,1'-bis-(diphenylphosphine)
촉매
HCID 6228Dimethylformamide용매
HCID 8857Ethyl Acetate용매

반응 조건

온도
120 °C

실험 절차

A mixture of trifluoromethanesulfonic acid 8-chloro-3-(4-chlorophenylsulfanyl)-2,4-dimethylquinolin-5-yl ester (0.31 g), tert-butyl-(1-methoxyvinyloxy)dimethyl silane (0.71 mL), sodium acetate (0.064 g), bis(dibenzylideneacetone) palladium (0.018 g) and 1,1′-bis(diphenylphospino) ferrocene (0) (0.018 g) in N,N-dimethylformamide (4.0 mL) was heated by microwave irradiation at 120° C. for 15 minutes. The mixture was diluted with ethyl acetate, and this solution was washed with saturated aqueous ammonium chloride solution and saturated aqueous sodium chloride solution and then dried over magnesium sulfate. The solvent was removed under reduced pressure and purification of the residue by column chromatography on silica gel, eluting with a mixture of dichloromethane and cyclohexane (1:1 to 2:0 by volume) gave title compound as a pale yellow solid, 0.15 g.

후처리

  1. washthis solution was washed with saturated aqueous ammonium chloride solution and saturated aqueous sodium chloride solution
  2. dry with materialdried over magnesium sulfate
  3. customThe solvent was removed under reduced pressure and purification of the residue by column chromatography on silica gel
  4. washeluting with a mixture of dichloromethane and cyclohexane (1:1 to 2:0 by volume)

출처 및 근거

ORD 기록
ord-b608b298808f4739a6d2622055a05eaa
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07858640B2

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