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Water → 4,4-Bis(3,7-dimethyloctyl)-dithieno[3,2-b:2',3'-d]silole

HRID 1504251
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HRID 1504251 반응식
Br[C:2]1[CH:6]=[C:5]([Si](C)(C)C)[S:4][C:3]=1[C:11]1[S:12][C:13]([Si](C)(C)C)=[CH:14][C:15]=1Br.C([Li])CCC.[CH3:26][CH:27]([CH2:43][CH2:44][CH2:45][CH:46]([CH3:48])[CH3:47])[CH2:28][CH2:29][Si:30]([CH2:33][CH2:34][CH:35]([CH3:42])[CH2:36][CH2:37][CH2:38][CH:39]([CH3:41])[CH3:40])(Cl)Cl.O>O1CCCC1.CCCCCC>[CH3:26][CH:27]([CH2:43][CH2:44][CH2:45][CH:46]([CH3:48])[CH3:47])[CH2:28][CH2:29][Si:30]1([CH2:33][CH2:34][CH:35]([CH3:42])[CH2:36][CH2:37][CH2:38][CH:39]([CH3:40])[CH3:41])[C:2]2[CH:6]=[CH:5][S:4][C:3]=2[C:11]2[S:12][CH:13]=[CH:14][C:15]1=2
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참가 물질

7

반응물 4

HCID 962WaterHCID 158605403,3'-Dibromo-5,5'-bis(trimethylsilyl)-2,2'-bithiopheneHCID 78062573Bis(3,7-dimethyloctyl)dichlorosilaneHCID 178418339Butyllithium

생성물 1

HCID 1239609394,4-Bis(3,7-dimethyloctyl)-dithieno[3,2-b:2',3'-d]silole수율 56%

시약·촉매·용매 2

HCID 8028
Tetrahydrofuran
용매
HCID 8058Hexane용매

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온도
-78 °C

실험 절차

3,3′-dibromo-5,5′-bis(trimethylsilyl)-2,2′-bithiophene (Compound G4, synthesized in accordance with WO 2010/136353, 11.6 g, 24.7 mmol) was placed in a 500 mL four-necked flask in a nitrogen atmosphere, and dissolved in tetrahydrofuran (200 mL). This was cooled to −78° C., and a solution of n-butyl lithium in hexane (KANTO CHEMICAL CO., INC., 1.59 M, 32.7 mL) was added dropwise. After about 20 minutes of agitation, the bis(3,7-dimethyloctyl)dichlorosilane (Compound G21, 11.3 g) synthesized in Synthesis Example B18 was added dropwise. The temperature was raised gradually to room temperature over the course of about 2 hours, water was added, and the product was extracted with hexane. The organic layer was washed with water, dried over sodium sulfate, and concentrated by filtration. The resulting oily substance was dissolved in chloroform (40 mL) and hexane (80 mL), trifluoroacetic acid (3.7 mL) was added, and the mixture was agitated for about 10 minutes at room temperature. Saturated sodium bicarbonate solution was added to the reaction solution, which was extracted with hexane and then concentrated under reduced pressure. The resulting yellow oily substance was dissolved in hexane, and subjected to silica gel column chromatography (solvent: hexane) to obtain the target 4,4-bis(3,7-dimethyloctyl)-dithieno[3,2-b:2′,3′-d]silole (Compound G22, 6.5 g, yield 56%.

후처리

  1. additionwas added dropwise
  2. additionwas added
  3. extractionthe product was extracted with hexane
  4. washThe organic layer was washed with water
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated by filtration
  7. dissolutionThe resulting oily substance was dissolved in chloroform (40 mL)
  8. additionhexane (80 mL), trifluoroacetic acid (3.7 mL) was added
  9. additionSaturated sodium bicarbonate solution was added to the reaction solution, which
  10. extractionwas extracted with hexane
  11. concentrationconcentrated under reduced pressure
  12. dissolutionThe resulting yellow oily substance was dissolved in hexane

출처 및 근거

ORD 기록
ord-dfb9f3b1cb1d4dc8a5f207b3faac4c75
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09212254B2

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