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

HRID 240215노트

반응식

HRID 240215 반응식
[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

참가 물질

5

반응물 2

HCID 109594842,6-DibromoanthraquinoneHCID 178506676HCID 178506676, 화합물

생성물 1

HCID 207305232,6-Dibromo-9,10-diphenylanthracene수율 67.5%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 3283Diethyl Ether용매2회

반응 조건

온도
130 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7918b93899364f3f9e5155c1d11dcbe8
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08647753B2

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