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

HRID 1914419
ノート
印刷プレビュー

反応式

HRID 1914419 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 2.6 g of 1,6-bis(4-methylphenyl)pyrene, 1.2 g of N-bromosuccinimide and 60 ml of dimethylformamide was stirred under a nitrogen gas stream at 60° C. for 5 hours. The solution was cooled to room temperature and 60 ml of water was poured into the solution, 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 resulting solid was recrystallized from toluene and then vacuum-dried to obtain 1.4 g of 3-bromo-1,6-bis(4-methylphenyl)pyrene.

後処理

  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 resulting solid was recrystallized from toluene
  6. customvacuum-dried

出典と根拠

ORDレコード
ord-7b3bc05721304183b2f1c9fb2f91b4a6
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08610345B2

反応ノート

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