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

HRID 600166
ノート
印刷プレビュー

反応式

HRID 600166 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0a4f29189bd14aec885d8427fa1c2860
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07901794B2

反応ノート

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