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Triphenylphosphine → HCID 59321561, 화합물

HRID 2423540
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HRID 2423540 반응식
Br[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:6]=[N:5]2.[Cl:17][C:18]1[CH:23]=[CH:22][CH:21]=[C:20]([Cl:24])[C:19]=1[C:25]1[C:29]([CH2:30][O:31][C:32]2[CH:37]=[CH:36][C:35](B3OC(C)(C)C(C)(C)O3)=[CH:34][CH:33]=2)=[C:28]([CH:47]([CH3:49])[CH3:48])[O:27][N:26]=1.P([O-])([O-])([O-])=O.[K+].[K+].[K+].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>ClCCl.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.O.O1CCOCC1>[Cl:24][C:20]1[CH:21]=[CH:22][CH:23]=[C:18]([Cl:17])[C:19]=1[C:25]1[C:29]([CH2:30][O:31][C:32]2[CH:33]=[CH:34][C:35]([C:2]3[CH:3]=[C:4]4[C:9](=[CH:10][CH:11]=3)[N:8]=[C:7]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:6]=[N:5]4)=[CH:36][CH:37]=2)=[C:28]([CH:47]([CH3:49])[CH3:48])[O:27][N:26]=1
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참가 물질

9

반응물 4

HCID 11776TriphenylphosphineHCID 62657Potassium Phosphate, TribasicHCID 59321593HCID 59321593, 화합물HCID 597090393-(2,6-Dichlorophenyl)-5-(1-methylethyl)-4-({[4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl]oxy}methyl)isoxazole

생성물 1

HCID 59321561HCID 59321561, 화합물수율 56%

시약·촉매·용매 4

HCID 167845palladium(II) acetate촉매HCID 962Water용매HCID 6344Dichloromethane용매HCID 312751,4-Dioxane용매

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온도
60 °C

실험 절차

Ethyl 6-bromo-2-quinoxalinecarboxylate (0.108 g, 0.384 mmol), 3-(2,6-dichlorophenyl)-5-(1-methylethyl)-4-({[4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl]oxy}methyl)isoxazole (0.27 g, 0.553 mmol), potassium phosphate (0.256 g, 1.21 mmol), palladium(II)acetate (0.0088 g, 0.039 mmol), triphenylphosphine (0.013 g, 0.050 mmol), 1,4-dioxane (8 mL) and water (0.035 mL) were combined and heated at 60° C. with stirring overnight. After 20 hours, the reaction mixture was allowed to stand at room temperature. The reaction mixture was partitioned between water and ethyl acetate. The aqueous phase was separated and extracted a second time with ethyl acetate. The organic extracts were combined, washed with brine, dried over magnesium sulfate, filtered, and the filtrate was concentrated to give an oil. The crude product was purified by flash chromatography over silica with hexanes:ethyl acetate (100:0 to 50:50) to give a yellow solid. The solid was dissolved in dichloromethane and the solution was concentrated to give 0.12 g (56%) of ethyl 6-[4-({[3-(2,6-dichlorophenyl)-5-(1-methylethyl)-4-isoxazolyl]methyl}oxy)phenyl]-2-quinoxalinecarboxylate as a yellow amorphous solid. 1H NMR (CDCl3, 400 MHz): δ 9.52 (s, 1H), 8.31 (d, J=9 Hz, 1H), 8.27 (d, J=2 Hz, 1H), 8.06 (dd, J=9, 2 Hz, 1H), 7.65 (d, J=9 Hz, 2H), 7.41 (m, 2H), 7.32 (dd, J=9, 7 Hz, 1H), 6.92 (d, J=9 Hz, 2H), 4.80 (s, 2H), 4.60 (quartet, J=7 Hz, 2H), 3.36 (septet, J=7 Hz, 1H), 1.51 (t, J=7 Hz, 3H), 1.44 (d, J=7 Hz, 6H). ESI-LCMS m/z 562 (M+H)+.

후처리

  1. waitAfter 20 hours
  2. customto stand at room temperature
  3. customThe reaction mixture was partitioned between water and ethyl acetate
  4. customThe aqueous phase was separated
  5. extractionextracted a second time with ethyl acetate
  6. washwashed with brine
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. concentrationthe filtrate was concentrated
  10. customto give an oil
  11. customThe crude product was purified by flash chromatography over silica with hexanes:ethyl acetate (100:0 to 50:50)
  12. customto give a yellow solid
  13. concentrationthe solution was concentrated

출처 및 근거

ORD 기록
ord-90c0946a28ea44bcae974ec4a3fd4bf6
출처 데이터셋
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07960552B2

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