Water → Dimethyl-bis(2-methyl-1H-inden-1-yl)silane

HRID 54608

反応式

HRID 54608 の反応式
[CH3:1][C:2]1[CH2:3][C:4]2[C:9]([CH:10]=1)=[CH:8][CH:7]=[CH:6][CH:5]=2.[CH3:11][Si:12]([CH3:15])(Cl)Cl.O>O1CCCC1.C([Li])CCC.CCCCCC>[CH3:11][Si:12]([CH3:15])([CH:10]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:3]=[C:2]1[CH3:1])[CH:3]1[C:4]2[C:9](=[CH:8][CH:7]=[CH:6][CH:5]=2)[CH:10]=[C:2]1[CH3:1]

参加物

7

反応物 3

HCID 962WaterHCID 6398DichlorodimethylsilaneHCID 165871H-Indene, 2-methyl-

生成物 1

HCID 4050248Dimethyl-bis(2-methyl-1H-inden-1-yl)silane収率 68%

試薬・触媒・溶媒 3

HCID 8028Tetrahydrofuran溶媒HCID 8058Hexane溶媒HCID 178418339Butyllithium溶媒

実験手順

In a 500 ml glass reactor, 4.3 g (33 mmole) of 2-methylindene was dissolved in 80 ml of tetrahydrofuran, to which 21 ml of 1.6M n-butyllithium in hexane was slowly added under cooling. After the mixture was stirred at room tempearture for 1 hour, it was cooled again, and 2.1 g of dimethyldichlorosilane was added dropwise. After the mixture was stirred at room temperature for 12 hours, 50 ml of water was added, and the organic phase was separated and dried to give 3.5 g of dimethylbis(2-methylindenyl)silane.

後処理

  1. additionwas slowly added
  2. temperatureunder cooling
  3. temperatureit was cooled again
  4. stirringAfter the mixture was stirred at room temperature for 12 hours
  5. customthe organic phase was separated
  6. customdried

出典と根拠

ORDレコード
ord-151018c2ea9f40899b919dffed3610ca
出典データセット
uspto-grants-1997_04
特許番号
US05623022

関連ノート

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