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

HRID 1457373노트

반응식

HRID 1457373 반응식
[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]

참가 물질

6

반응물 3

HCID 7076M-TerphenylHCID 5359268AluminumHCID 19360808(2,2-Dichloroethyl)trichlorosilane

생성물 1

HCID 221046119-(Trichlorosilyl)methyl-3-phenylfluorene수율 15%

시약·촉매·용매 2

HCID 6348Carbon Disulfide용매HCID 8058Hexane용매2회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-3337652cacb9499eb32a75a6e0e96bf7
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05847182

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