4-Bromobiphenyl → 2-Bromo-9-(trichlorosilyl)methylfluorene

HRID 1457374

反応式

HRID 1457374 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.[Al].Cl[CH:16](Cl)[CH2:17][Si:18]([Cl:21])([Cl:20])[Cl:19]>C(=S)=S.CCCCCC>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[C:8]3[C:13](=[CH:12][CH:11]=[CH:10][CH:9]=3)[CH:16]([CH2:17][Si:18]([Cl:21])([Cl:20])[Cl:19])[C:6]=2[CH:7]=1

参加物

6

反応物 3

HCID 71014-BromobiphenylHCID 5359268AluminumHCID 19360808(2,2-Dichloroethyl)trichlorosilane

生成物 1

HCID 221046082-Bromo-9-(trichlorosilyl)methylfluorene収率 15%

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 4-bromobiphenyl and 0.08 g (11.1 mmol) of aluminum foil were alkylated in CS2 (50 ml) solution with (2,2-dichloroethyl)-trichlorosilane 6.68 g (21.7 mmol) for 24 hr. 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, the reaction products were vacuum distilled to give 1.28 g of 2-bromo-9-(trichlorosilyl)methylfluorene (yield; 15%).

後処理

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

出典と根拠

ORDレコード
ord-0d8ec0c8224946758190bb6acad92d0b
出典データセット
uspto-grants-1998_12
特許番号
US05847182

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