Dichlorodimethylsilane → 9,10-Bis(chlorodimethylsilyl)anthracene

HRID 49746

反応式

HRID 49746 の反応式
[Li][C:2]1[C:3]2[C:8]([C:9]([Li])=[C:10]3[C:15]=1[CH:14]=[CH:13][CH:12]=[CH:11]3)=[CH:7][CH:6]=[CH:5][CH:4]=2.Cl[Si:18]([Cl:21])([CH3:20])[CH3:19]>C(OCC)C>[Cl:21][Si:18]([CH3:20])([CH3:19])[C:2]1[C:3]2[C:8]([C:9]([Si:18]([Cl:21])([CH3:20])[CH3:19])=[C:10]3[C:15]=1[CH:14]=[CH:13][CH:12]=[CH:11]3)=[CH:7][CH:6]=[CH:5][CH:4]=2

参加物

4

反応物 2

HCID 6398DichlorodimethylsilaneHCID 178506633HCID 178506633、化合物

生成物 1

HCID 227415949,10-Bis(chlorodimethylsilyl)anthracene収率 13%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

The obtained solution of 9,10-dilithioanthracene was dropped into a solution prepared from 61.4 g (0.476 mol) of dichlorodimethylsilane and 40 ml of dried diethyl ether as a solvent, in a 1L-volume flask for 2 hours using a separating funnel. After the solution was stirred for 44 hours at room temperature and salt yielded by reaction was removed by means of filtration, the remaining filtrate was concentrated to remove the solvent of the filtrate using an evaporator. The residue was recrystallized in n-pentane to obtain 5.6 g (yield: 13%) of yellow 9,10-bis(chlorodimethylsilyl)anthracene.

後処理

  1. customsalt yielded by reaction
  2. customwas removed by means of filtration
  3. concentrationthe remaining filtrate was concentrated
  4. customto remove the solvent of the filtrate
  5. customan evaporator
  6. customThe residue was recrystallized in n-pentane

出典と根拠

ORDレコード
ord-1b1bc7f1794f48499d07ff8fe9b3ca90
出典データセット
uspto-grants-2004_03
特許番号
US06709772B2

関連ノート

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