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Dimethylformamide → 3-Bromo-1,6-bis(4-methylphenyl)pyrene

HRID 600166
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HRID 600166 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:21]3[C:22]4=[C:23]5[C:18](=[CH:19][CH:20]=3)[CH:17]=[CH:16][C:15]([C:24]3[CH:29]=[CH:28][C:27]([CH3:30])=[CH:26][CH:25]=3)=[C:14]5[CH:13]=[CH:12][C:11]4=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.[Br:31]N1C(=O)CCC1=O.CN(C)C=O>O>[Br:31][C:17]1[CH:16]=[C:15]([C:24]2[CH:29]=[CH:28][C:27]([CH3:30])=[CH:26][CH:25]=2)[C:14]2[C:23]3=[C:22]4[C:11]([CH:10]=[CH:9][C:8]([C:5]5[CH:4]=[CH:3][C:2]([CH3:1])=[CH:7][CH:6]=5)=[C:21]4[CH:20]=[CH:19][C:18]=13)=[CH:12][CH:13]=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 67184N-bromobutanimideHCID 207305171,6-Bis(4-methylphenyl)pyrene

생성물 1

HCID 866285953-Bromo-1,6-bis(4-methylphenyl)pyrene수율 45%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Next, a mixed solution of 1.3 g of 1,6-bis(4-methylphenyl)pyrene, 0.6 g of N-bromosuccinimide and 30 ml of dimethylformamide was stirred under nitrogen gas stream at a temperature of 60° C. for 5 hours. After cooling the mixed solution to room temperature, 30 ml of water was injected thereinto to extract therefrom with 100 ml of dichloromethane. The organic layer was washed twice with 50 ml of water, dried by magnesium sulfate and thereafter evaporated. The organic layer was recrystallized from toluene and vacuum dried to thereafter obtain 0.7 g of 3-bromo-1,6-bis(4-methylphenyl)pyrene.

후처리

  1. extractionto extract
  2. washThe organic layer was washed twice with 50 ml of water
  3. dry with materialdried by magnesium sulfate
  4. customevaporated
  5. customThe organic layer was recrystallized from toluene and vacuum
  6. customdried

출처 및 근거

ORD 기록
ord-0a4f29189bd14aec885d8427fa1c2860
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07901794B2

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