M-Terphenyl → 9-(Trichlorosilyl)methyl-3-phenylfluorene

HRID 1457373ノート

反応式

HRID 1457373 の反応式
[C:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[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:12]2[CH:11]=[CH:10][C:9]([C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=3)=[CH:8][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 7076M-TerphenylHCID 5359268AluminumHCID 19360808(2,2-Dichloroethyl)trichlorosilane

生成物 1

HCID 221046119-(Trichlorosilyl)methyl-3-phenylfluorene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 meta-terphenyl and 0.47 g (17.4 mmol) of aluminum foil 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 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, recrystallization from ether yielded 1.27 g of 9-(trichlorosilyl)methyl-3-phenylfluorene (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. customrecrystallization from ether

出典と根拠

ORDレコード
ord-3337652cacb9499eb32a75a6e0e96bf7
出典データセット
uspto-grants-1998_12
特許番号
US05847182

反応ノート

読み込み中…