Dichlorodimethylsilane → Dimethyl(2-methylindenyl)silyl chloride

HRID 1953958ノート

反応式

HRID 1953958 の反応式
[CH3:1][Si:2]([CH3:5])(Cl)[Cl:3].O1CCCC1.[CH3:11][C:12]1[CH:13]([Li])[C:14]2[C:19]([CH:20]=1)=[CH:18][CH:17]=[CH:16][CH:15]=2>CCCCCC>[CH3:1][Si:2]([Cl:3])([CH3:5])[CH:13]1[C:14]2[C:19](=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH:20]=[C:12]1[CH3:11]

参加物

5

反応物 3

HCID 6398DichlorodimethylsilaneHCID 8028TetrahydrofuranHCID 178506826HCID 178506826、化合物

生成物 1

HCID 21943870Dimethyl(2-methylindenyl)silyl chloride収率 58%

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

In a three-necked flask equipped with a mechanical stirrer were charged 44.5 g (345 mmol) of dimethyldichlorosilane, 300 ml of tetrahydrofuran and n-hexane, to which was added at -78° C. a 2-methylindenyllithium solution, followed by stirring at room temperature for 3 hours. After the solvent was distilled off under reduced pressure, 100 ml of hexane was added and insoluble matter was removed by centrifugation. After the solvent was distilled off under reduced pressure, distillation under reduced pressure (113° C./7mmHg) afforded 14.9 g (67 mmol, yield: 58%) of dimethyl(2-methylindenyl)silyl chloride as a pale yellow liquid.

後処理

  1. customIn a three-necked flask equipped with a mechanical stirrer
  2. distillationAfter the solvent was distilled off under reduced pressure, 100 ml of hexane
  3. additionwas added
  4. custominsoluble matter was removed by centrifugation
  5. distillationAfter the solvent was distilled off under reduced pressure, distillation under reduced pressure (113° C./7mmHg)

出典と根拠

ORDレコード
ord-ae69011f711b4342ba0c54b65629a3c9
出典データセット
uspto-grants-2000_09
特許番号
US06121182

反応ノート

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