Water → 5,8-Dibromo-2,3-diphenylquinoxaline

HRID 533584

반응식

HRID 533584 반응식
[Br:1][C:2]1[C:3]([NH2:10])=[C:4]([NH2:9])[C:5]([Br:8])=[CH:6][CH:7]=1.[C:11]1([C:17]([C:19]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=O)=O)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.O.C(=O)(O)[O-].[Na+]>C(O)(=O)C>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([Br:8])=[C:4]2[C:3]=1[N:10]=[C:17]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[C:19]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)=[N:9]2

참가 물질

6

반응물 4

HCID 962WaterHCID 8651BenzilHCID 516892Sodium BicarbonateHCID 118215323,6-Dibromobenzene-1,2-diamine

생성물 1

HCID 224759015,8-Dibromo-2,3-diphenylquinoxaline

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

The detailed preparation procedure is as follows: 3,6-dibromo-o-phenylene diamine (1.0 g, 3.7 mmol) was added to a solution of compound benzil (0.39 g, 1.84 mmol) in acetic acid (20 mL) at 120□, then the mixture was mixed uniformly. After refluxed for 12 hours, the fluid reactant was poured into water, and neutralized with sodium bicarbonate until neutral, then extracted with chloroform and washed with saturated brine, dried over anhydrous sodium sulfate, then it was vacuum evaporated to remove the solvent, and the resulting crude product was purified by column chromatography to give a white solid, and then it was purified by recrystallization from chloroform/n-hexane to give a white solid powder. The test result is: MS (EI) m/z: 440(M+).

후처리

  1. customThe detailed preparation procedure
  2. additionthe mixture was mixed uniformly
  3. temperatureAfter refluxed for 12 hours
  4. extractionthen extracted with chloroform
  5. washwashed with saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. customevaporated
  8. customto remove the solvent
  9. customthe resulting crude product was purified by column chromatography
  10. customto give a white solid
  11. customit was purified by recrystallization from chloroform/n-hexane
  12. customto give a white solid powder
  13. customThe test result

출처 및 근거

ORD 기록
ord-036f8be6036b4223b33192d6e1f3491f
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08853348B2

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