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

HRID 1457374

반응식

HRID 1457374 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 221046082-Bromo-9-(trichlorosilyl)methylfluorene수율 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 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%).

후처리

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

출처 및 근거

ORD 기록
ord-0d8ec0c8224946758190bb6acad92d0b
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05847182

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