2(1H)-Quinoxalinone → 6-Bromo-1,2-dihydroquinoxalin-2-one

HRID 1020732노트

반응식

HRID 1020732 반응식
[NH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]=[CH:3][C:2]1=[O:11].[Br:12]Br>S(=O)(=O)(O)O.C(Cl)(Cl)(Cl)Cl.S([O-])([O-])(=O)=O.[Ag+2]>[Br:12][C:7]1[CH:6]=[C:5]2[C:10](=[CH:9][CH:8]=1)[NH:1][C:2](=[O:11])[CH:3]=[N:4]2

참가 물질

6

반응물 2

HCID 145262(1H)-QuinoxalinoneHCID 24408Bromine

생성물 1

HCID 126863946-Bromo-1,2-dihydroquinoxalin-2-one수율 40%

시약·촉매·용매 3

HCID 178418844HCID 178418844, 화합물촉매HCID 1118Sulfuric Acid용매HCID 5943Carbon Tetrachloride용매

반응 조건

온도
50 °C

실험 절차

The quinoxalin-2(1H)-one (14.6 g, 0.1 mol, Aldrich, cat. no. 260517) and silver sulphate (15.6 g, 0.05 mol) were dissolved in conc. Sulfuric acid (100 ml) at 20° C. Bromine (5.2 ml, 0.1 mol) was added and the reaction mixture was stirred vigorously for 24 hours. The reaction mass was then diluted with carbon tetrachloride (100 mL), and this was heated at 50° C. The reaction mass was then filtered and the filtrate was poured into ice cold water and stirred for 30 minutes to obtain a precipitate. The precipitate was filtered and the solid material was dried in vacuo to afford the title product (9.0 g, 40%).

후처리

  1. filtrationThe reaction mass was then filtered
  2. additionthe filtrate was poured into ice cold water
  3. stirringstirred for 30 minutes
  4. customto obtain a precipitate
  5. filtrationThe precipitate was filtered
  6. customthe solid material was dried in vacuo

출처 및 근거

ORD 기록
ord-aee6e2da2807442db7911757998664ff
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08716473B2

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