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

HRID 2253255

反応式

HRID 2253255 の反応式
[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.C([O-])(=O)C.[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

参加物

5

反応物 3

HCID 8651BenzilHCID 517045Sodium AcetateHCID 118215323,6-Dibromobenzene-1,2-diamine

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 5.3 g (20 mmol) of 3,6-dibromo-1,2-phenylenediamine 1, 4 g (19 mmol) of benzil 2b, 4.2 g of sodium acetate and 150 ml of glacial acetic acid were refluxed for 4 hours. The precipitate was filtered off, washed with 100 ml of water and recrystallized twice from dioxane. Drying under reduced pressure at 50° C. gave the pure product in the form of colorless crystals, which according to HPLC had a purity of about 99.5%. The yield was 6.45 g (73%).

後処理

  1. filtrationThe precipitate was filtered off
  2. washwashed with 100 ml of water
  3. customrecrystallized twice from dioxane
  4. customDrying under reduced pressure at 50° C.
  5. customgave the pure product in the form of colorless crystals, which

出典と根拠

ORDレコード
ord-d2b26941111d424eadb4ed323447c7db
出典データセット
uspto-grants-2008_01
特許番号
US07323533B2

関連ノート

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