2,6-Dibromoanthraquinone → 2,6-Dibromo-9,10-diphenylanthracene

HRID 240215ノート

反応式

HRID 240215 の反応式
[C:1]1([Li])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Br:8][C:9]1[CH:22]=[CH:21][C:20]2[C:19](=O)[C:18]3[C:13](=[CH:14][CH:15]=[C:16]([Br:24])[CH:17]=3)[C:12](=O)[C:11]=2[CH:10]=1>CCOCC.CC(O)=O>[Br:8][C:9]1[CH:22]=[CH:21][C:20]2[C:11](=[C:12]([C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)[C:13]3[C:18]([C:19]=2[C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)=[CH:17][C:16]([Br:24])=[CH:15][CH:14]=3)[CH:10]=1

参加物

5

反応物 2

HCID 109594842,6-DibromoanthraquinoneHCID 178506676HCID 178506676、化合物

生成物 1

HCID 207305232,6-Dibromo-9,10-diphenylanthracene収率 67.5%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 3283Diethyl Ether溶媒2 回

反応条件

温度
130 °C

実験手順

6 g of phenyl lithium was dissolved in Et2O, and the resulting solution was gradually added dropwise to a solution containing 5 g of 2,6-dibromoanthraquinone dissolved in Et2O. This reaction was carried out on a dry ice bath. Then, the temperature of the reaction material was elevated to room temperature, thereby obtaining white solids. The obtained solids were dissolved in 100 mL of AcOH, followed by addition of KI and NaH2PO2 and the resulting mixture was stirred at 130° C. for 24 hours. After the reaction was complete, the resulting material was filtered with addition of water. The filtrate was then recrystallized from MC and MeOH, thereby obtaining 4.5 g of 2,6-dibromo-9,10-diphenylanthracene.

後処理

  1. additionthe resulting solution was gradually added dropwise to a solution
  2. customThis reaction was carried out on a dry ice bath
  3. customwas elevated to room temperature
  4. customobtaining white solids
  5. filtrationthe resulting material was filtered with addition of water
  6. customThe filtrate was then recrystallized from MC and MeOH

出典と根拠

ORDレコード
ord-7918b93899364f3f9e5155c1d11dcbe8
出典データセット
uspto-grants-2014_02
特許番号
US08647753B2

反応ノート

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