Fluorene → n-Hexylmethylbis(9-fluorenyl)silane

HRID 1957760노트

반응식

HRID 1957760 반응식
[CH2:1]([Si:7]([CH3:10])(Cl)Cl)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].[CH:11]1[C:23]2[CH2:22][C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[C:15]=2[CH:14]=[CH:13][CH:12]=1>C1COCC1>[CH2:1]([Si:7]([CH3:10])([CH:22]1[C:23]2[CH:11]=[CH:12][CH:13]=[CH:14][C:15]=2[C:16]2[C:21]1=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:22]1[C:21]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[C:15]2[C:23]1=[CH:11][CH:12]=[CH:13][CH:14]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6]

참가 물질

4

반응물 2

HCID 6853Fluorene2회HCID 84650Hexylmethyldichlorosilane

생성물 1

HCID 22623330n-Hexylmethylbis(9-fluorenyl)silane

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

n-Hexylmethyldichlorosilane (30.4 g, 0.152 mol) and 300 mL of dry THF were charged to a one liter Schlenk equipped with an addition funnel. Fluorene anion (52.4 g, 0.305 mol) was dissolved in approximately 200 mL of dry THF and charged to the addition funnel. The temperature of the stirring solution was lowered to -78° C. under positive nitrogen pressure. The fluorene anion was added dropwise over two hours. After the anion addition was complete, the reaction mixture was allowed to warm to room temperature. The solution was allowed to stir overnight. The solution was washed with three 200 mL aliquots of water, retaining the organic layer after each washing. The organic layer was dried with magnesium sulfate and filtered. The product was recrystallized from hexane. The yield of this reaction is 19.6%.

후처리

  1. customequipped with an addition funnel
  2. additioncharged to the addition funnel
  3. customwas lowered to -78° C. under positive nitrogen
  4. additionAfter the anion addition
  5. washThe solution was washed with three 200 mL aliquots of water
  6. dry with materialThe organic layer was dried with magnesium sulfate
  7. filtrationfiltered
  8. customThe product was recrystallized from hexane

출처 및 근거

ORD 기록
ord-aa4ec8095dc94e3ca39ff02f7e86a7e2
출처 데이터셋
uspto-grants-1998_07
특허 번호
US05786495

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