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

HRID 1020732ノート

反応式

HRID 1020732 の反応式
[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

参加物

6

反応物 2

HCID 145262(1H)-QuinoxalinoneHCID 24408Bromine

生成物 1

HCID 126863946-Bromo-1,2-dihydroquinoxalin-2-one収率 40%

試薬・触媒・溶媒 3

HCID 178418844HCID 178418844、化合物触媒HCID 1118Sulfuric Acid溶媒HCID 5943Carbon Tetrachloride溶媒

反応条件

温度
50 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-aee6e2da2807442db7911757998664ff
出典データセット
uspto-grants-2014_05
特許番号
US08716473B2

反応ノート

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