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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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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
ノート
印刷プレビュー

反応式

HRID 1446362 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-7b7068abfc444bd6a8711119d8d0a200
出典データセット
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07667064B2

反応ノート

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