9-(2-bromoethyl)-9H-fluorene → HCID 86752827, 화합물

HRID 1955286

반응식

HRID 1955286 반응식
[CH:1]([C:3]1[CH:15]=[CH:14][C:13]2[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[CH2:6][C:5]=2[CH:4]=1)=[CH2:2].C([Li])CCC.Br[CH2:22][CH2:23][CH:24]1[C:36]2[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=2[C:30]2[C:25]1=[CH:26][CH:27]=[CH:28][CH:29]=2>C(OCC)C>[CH:1]([C:3]1[CH:15]=[CH:14][C:13]2[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[CH2:6][C:5]=2[C:4]=1[C:24]1([CH2:23][CH3:22])[C:36]2[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=2[C:30]2[C:25]1=[CH:26][CH:27]=[CH:28][CH:29]=2)=[CH2:2]

참가 물질

5

반응물 3

HCID 110002159-(2-bromoethyl)-9H-fluoreneHCID 110416072-ethenyl-9H-fluoreneHCID 178418339Butyllithium

생성물 1

HCID 86752827HCID 86752827, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To 1.15 g (6.0 mmol) 2-vinylfluorene in 100 mL diethyl ether was added 3.75 mL (6.0 mmol) n-butyllithium (1.6M in hexane). The reaction mixture was stirred for 4 hours at room temperature. Then 1.64 g (6.0 mmol) 1-bromo-2-(9-fluorenyl)ethane was added and the mixture was stirred for 14 hours at room temperature. The precipitate was removed by filtration, washed with methanol, filtered with pentane using silica gel 60, and concentrated by evaporation under vacuum. The yield was 1.69 g (73%) 1-(9-(2-vinyl)fluorenyl)-2-(9-fluorenyl)ethane as a colorless solid.

후처리

  1. stirringthe mixture was stirred for 14 hours at room temperature
  2. customThe precipitate was removed by filtration
  3. washwashed with methanol
  4. filtrationfiltered with pentane
  5. concentrationconcentrated by evaporation under vacuum

출처 및 근거

ORD 기록
ord-188e5440bfd343b7bbf8113769096646
출처 데이터셋
uspto-grants-2000_09
특허 번호
US06124414

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