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2,5-Dibromo-3,4-dimethylthieno[2,3-b]thiophene → HCID 23070268, 화합물

HRID 351298
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HRID 351298 반응식
Br[C:2]1[S:11][C:5]2[S:6][C:7](Br)=[C:8]([CH3:9])[C:4]=2[C:3]=1[CH3:12].B([O-])[O-].[CH2:16]([C:22]1[CH:23]=[CH:24][S:25][CH:26]=1)[CH2:17][CH2:18][CH2:19][CH2:20][CH3:21].[Na+].[Na+].[Na]>COCCOC.C(OCC)C>[CH2:16]([C:22]1[CH:23]=[C:24]([C:2]2[S:11][C:5]3[S:6][C:7]([C:24]4[S:25][CH:26]=[C:22]([CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])[CH:23]=4)=[C:8]([CH3:9])[C:4]=3[C:3]=2[CH3:12])[S:25][CH:26]=1)[CH2:17][CH2:18][CH2:19][CH2:20][CH3:21]
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참가 물질

6

반응물 3

HCID 28201622,5-Dibromo-3,4-dimethylthieno[2,3-b]thiopheneHCID 5360545SodiumHCID 178442413HCID 178442413, 화합물

생성물 1

HCID 23070268HCID 23070268, 화합물

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 80711,2-Dimethoxyethane용매

실험 절차

To a solution of 2,5-dibromo-3,4-dimethylthieno[2,3-b]thiophene (3.02 g, 9.28 mmol) and sodium 4-hexylthiophene boronate (5.14 g, 20.4 mmol) in degassed DME (200 ml) was added tetrakis(triphenyl-phosphine)palladium(0) (0.5 g, 5 mol %). The solution was heated to reflux and a saturated solution of sodium hyodrogen carbonate (4.2 g, 49 mmol) was added slowly. The reaction was refluxed for 16 h, cooled and diluted with diethyl ether. The layers were separated and the organics washed with 5% HCl, brine, dried (Na2SO4), filtered and concentrated under reduced pressure. The crude product was purified by column chromatography over silica (eluent: petrol) to afford the product after recrystallisation from petroi (1.03 g, 22%). :M/Z 500 (M+). Found C, 66.9.1, H, 6.9, S, 25.3. Calc. for C28H36S4 C, 67.2; H 7.2, S, 25.6. NMR gave the expected signals.

후처리

  1. temperatureThe solution was heated
  2. temperatureto reflux
  3. temperatureThe reaction was refluxed for 16 h
  4. temperaturecooled
  5. customThe layers were separated
  6. washthe organics washed with 5% HCl, brine
  7. dry with materialdried (Na2SO4)
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure
  10. customThe crude product was purified by column chromatography over silica (eluent: petrol)
  11. customto afford the product
  12. customafter recrystallisation from petroi (1.03 g, 22%)
  13. customNMR gave the expected signals

출처 및 근거

ORD 기록
ord-cc216c3dd21040b7992e4494986f7e52
출처 데이터셋
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07183418B2

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