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

HRID 1027316
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HRID 1027316 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 64.3%

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 a nitrogen gas flow at 60° C. for 5 hours. After cooling the solution to room temperature, 30 ml of water was injected, followed by extraction with 100 ml of dichloromethane. The organic layer was washed twice with 50 ml of water, dried over magnesium sulfate and then evaporated. The resultant solid was recrystallized from toluene and then vacuum-dried to obtain 1.0 g of 3-bromo-1,6-bis(4-methylphenyl)pyrene.

후처리

  1. extractionfollowed by extraction with 100 ml of dichloromethane
  2. washThe organic layer was washed twice with 50 ml of water
  3. dry with materialdried over magnesium sulfate
  4. customevaporated
  5. customThe resultant solid was recrystallized from toluene
  6. customvacuum-dried

출처 및 근거

ORD 기록
ord-12b2abdae74b4718a7efbb81c4d1bb41
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08729530B2

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