p-Terphenyl → 9-(Trichlorosilyl)methyl-2-phenylfluorene

HRID 1457372

反応式

HRID 1457372 の反応式
[C:1]1([C:7]2[CH:12]=[CH:11][C:10]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)=[CH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Al].Cl[CH:21](Cl)[CH2:22][Si:23]([Cl:26])([Cl:25])[Cl:24]>C(=S)=S.CCCCCC>[Cl:24][Si:23]([CH2:22][CH:21]1[C:8]2[CH:9]=[C:10]([C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=3)[CH:11]=[CH:12][C:7]=2[C:1]2[C:2]1=[CH:3][CH:4]=[CH:5][CH:6]=2)([Cl:26])[Cl:25]

参加物

6

反応物 3

HCID 7115p-TerphenylHCID 5359268AluminumHCID 19360808(2,2-Dichloroethyl)trichlorosilane

生成物 1

HCID 221046079-(Trichlorosilyl)methyl-2-phenylfluorene収率 10%

試薬・触媒・溶媒 2

HCID 6348Carbon Disulfide溶媒HCID 8058Hexane溶媒2 回

実験手順

In the same apparatus and procedures as Example 1 above, 5.0 g (21.7 mmol) of para-terphenyl and 0.30 g (11.1 mmol) of aluminum were alkylated in CS2 (50 ml) solution with (2,2-dichloroethyl)trichlorosilane 6.68 g (21.7 mmol) under dry nitrogen atmospheric pressure for 24 hrs at reflux temperature. Freshly distilled hexane (100 ml) was added to the reaction mixture and insoluble solids in hexane were filtered from the organic solution. After hexane and CS2 were distilled, recrystallization from ether yielded 0.85 g of 9-(trichlorosilyl)methyl-2-phenylfluorene (yield; 10%).

後処理

  1. customfor 24 hrs
  2. temperatureat reflux temperature
  3. filtrationwere filtered from the organic solution
  4. distillationAfter hexane and CS2 were distilled
  5. customrecrystallization from ether

出典と根拠

ORDレコード
ord-44b5a1b2074441da9cd95f33c059751f
出典データセット
uspto-grants-1998_12
特許番号
US05847182

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