Indene → Dimesitylbis(indenyl)silane

HRID 1306

反応式

HRID 1306 の反応式
[CH2:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:3]=[CH:2]1.[CH2:10]([Li])[CH2:11][CH2:12][CH3:13].[C:15]1([CH3:35])[CH:20]=[C:19]([CH3:21])[CH:18]=[C:17]([CH3:22])[C:16]=1[Si:23]([C:26]1[C:31]([CH3:32])=[CH:30][C:29]([CH3:33])=[CH:28][C:27]=1[CH3:34])(Cl)Cl>C1COCC1>[C:15]1([CH3:35])[CH:20]=[C:19]([CH3:21])[CH:18]=[C:17]([CH3:22])[C:16]=1[Si:23]([C:26]1[C:31]([CH3:32])=[CH:30][C:29]([CH3:33])=[CH:28][C:27]=1[CH3:34])([CH:10]1[C:8]2[C:13](=[CH:3][CH:2]=[CH:1][CH:9]=2)[CH:12]=[CH:11]1)[CH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:3]=[CH:2]1

参加物

5

反応物 3

HCID 7219IndeneHCID 11404964DimesityldichlorosilaneHCID 178418339Butyllithium

生成物 1

HCID 19695123Dimesitylbis(indenyl)silane

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

7 g of indene in 50 cm3of THF were reacted with 24 cm3 of butyllithium (2.5-molar in hexane) at 0° C. under inert conditions. The mixture was heated to room temperature, added dropwise to a solution of 10 g of dimesityldichlorosilane in 40 cm3 of THF, and the mixture was refluxed for 4 hours. Decomposition of the batch with water, extraction with diethyl ether and chromatography on SiO2 using 2:1 toluene/hexane gave 3.28 g of dimesitylbis(indenyl)silane as a solid. MS(m/e,I rel %): 496 (100, M+); 1H NMR in CDCl3 : 2.22 ppm (12 H, s), 2.27 ppm (6 H, s), 3.40 ppm (4 H, s), 6.8-7.4 ppm (14 H, m).

後処理

  1. temperaturethe mixture was refluxed for 4 hours
  2. extractionDecomposition of the batch with water, extraction with diethyl ether and chromatography on SiO2 using 2:1 toluene/hexane

出典と根拠

ORDレコード
ord-68a3f07b1c044ef79787604ed33c105d
出典データセット
uspto-grants-1998_03
特許番号
US05723705

関連ノート

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