홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Water → 4H-Silolo[3,2-b:4,5-b']dithiophene, 4,4-didecyl-

HRID 1772570
노트
인쇄 미리보기

반응식

HRID 1772570 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.Cl[Si:27](Cl)([CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH3:47])[CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH3:37].O>O1CCCC1.CCCCCC>[CH2:38]([Si:27]1([CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH3:37])[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)[CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH3:47]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 158605403,3'-Dibromo-5,5'-bis(trimethylsilyl)-2,2'-bithiophene2회HCID 21889368Dichloro(didecyl)silaneHCID 178418339Butyllithium

생성물 1

HCID 1233927074H-Silolo[3,2-b:4,5-b']dithiophene, 4,4-didecyl-수율 88%

시약·촉매·용매 2

HCID 8028
Tetrahydrofuran
용매
HCID 8058Hexane용매

반응 조건

온도
-78 °C

실험 절차

3,3′-dibromo-5,5′-bis(trimethylsilyl)-2,2′-bithiophene (Compound E4, synthesized in accordance with WO 2010/136353, 5.0 g) was placed in a 200 mL four-necked flask in a nitrogen atmosphere, and dissolved in tetrahydrofuran (75 mL). This was cooled to −78° C., and a solution of n-butyl lithium in hexane (KANTO CHEMICAL CO., INC., 1.64 M, 13.7 mL) was added dropwise. After about 30 minutes of agitation, the dichlorodi-n-decylsilane (Compound E21) (4.89 g) synthesized in Synthesis Example A19 was added dropwise. The temperature was gradually raised to room temperature over the course of about 2 hours, after which water was added, and the product was extracted with hexane. The organic layer was washed with water, dried with anhydrous sodium sulfate, and concentrated by filtration. The resulting yellow-orange oily substance was dissolved in hexane (50 mL) and chloroform (25 mL), trifluoroacetic acid (2.2 mL) was added with the internal temperature at 2° C., and after 10 minutes of agitation water was added, and the organic layer was washed, dried with anhydrous sodium sulfate and then and concentrated by filtration. Heptane (32 mL) was added to the reaction solution, which was then concentrated under reduced pressure. The resulting yellow-green oily substance was dissolved in hexane, and subjected to silica gel column chromatography (solvent: hexane) to obtain the target 4,4-di-n-decyl-dithieno[3,2-b:2′,3′-d]silole (Compound E22, 4.46 g, yield 88%).

후처리

  1. additionwas added dropwise
  2. temperatureThe temperature was gradually raised to room temperature over the course of about 2 hours
  3. extractionthe product was extracted with hexane
  4. washThe organic layer was washed with water
  5. dry with materialdried with anhydrous sodium sulfate
  6. concentrationconcentrated by filtration
  7. dissolutionThe resulting yellow-orange oily substance was dissolved in hexane (50 mL)
  8. additionchloroform (25 mL), trifluoroacetic acid (2.2 mL) was added with the internal temperature at 2° C.
  9. additionafter 10 minutes of agitation water was added
  10. washthe organic layer was washed
  11. dry with materialdried with anhydrous sodium sulfate
  12. concentrationconcentrated by filtration
  13. additionHeptane (32 mL) was added to the reaction solution, which
  14. concentrationwas then concentrated under reduced pressure
  15. dissolutionThe resulting yellow-green oily substance was dissolved in hexane

출처 및 근거

ORD 기록
ord-d62737c0e1754a369528025c7b4bdd37
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09249257B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트