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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Chlorodimethyl(2,3,4,5-tetramethyl-2,4-cyclopentadien-1-yl)silane → N-(4-Bromo-2,6-diisopropylphenyl)(dimethyl)(2,3,4,5-tetramethyl-2,4-cyclopentadien-1-yl)silanamine

HRID 1446362
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HRID 1446362 반응식
[Br:1][C:2]1[CH:8]=[C:7]([CH:9]([CH3:11])[CH3:10])[C:5]([NH2:6])=[C:4]([CH:12]([CH3:14])[CH3:13])[CH:3]=1.[Li]CCCC.Cl[Si:21]([CH3:32])([CH3:31])[CH:22]1[C:26]([CH3:27])=[C:25]([CH3:28])[C:24]([CH3:29])=[C:23]1[CH3:30]>C1COCC1>[Br:1][C:2]1[CH:8]=[C:7]([CH:9]([CH3:10])[CH3:11])[C:5]([NH:6][Si:21]([CH3:31])([CH3:32])[CH:22]2[C:26]([CH3:27])=[C:25]([CH3:28])[C:24]([CH3:29])=[C:23]2[CH3:30])=[C:4]([CH:12]([CH3:14])[CH3:13])[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

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HCID 5045335Chlorodimethyl(2,3,4,5-tetramethyl-2,4-cyclopentadien-1-yl)silaneHCID 117801144-Bromo-2,6-diisopropylanilineHCID 178418339Butyllithium

생성물 1

HCID 58897738N-(4-Bromo-2,6-diisopropylphenyl)(dimethyl)(2,3,4,5-tetramethyl-2,4-cyclopentadien-1-yl)silanamine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

Under an argon atmosphere, to a solution of 13.8 g (53 mmol) of 4-bromo-2,6-diisopropylaniline in 170 ml of THF, 21.0 ml of 2.5 M (53 mmol) of nBuLi in hexanes were added dropwise at −80° C. This mixture was additionally stirred for 30 minutes at ambient temperature and then added to a solution of 11.4 g (53 nimol) of chloro(dimethyl)(2,3,4,5-tetramethyl-2,4-cyclopentadien-1-yl)silane in 70 ml of THF. The resulting mixture was stirred overnight and then evaporated to dryness. The residue was suspended in 100 ml of toluene. This suspension was filtered through a glass frit (G4). The filtrate was evaporated to dryness. Fractional distillation gave a yellow oil, b.p. 156-162° C./0.15 mm Hg. Yield 12.8 g (55%).

후처리

  1. stirringThe resulting mixture was stirred overnight
  2. customevaporated to dryness
  3. filtrationThis suspension was filtered through a glass frit (G4)
  4. customThe filtrate was evaporated to dryness
  5. distillationFractional distillation
  6. customgave a yellow oil, b.p. 156-162° C./0.15 mm Hg

출처 및 근거

ORD 기록
ord-7b7068abfc444bd6a8711119d8d0a200
출처 데이터셋
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07667064B2

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