Sodium Hydroxide → 6-Amino-5-bromoquinoxaline hydrobromide

HRID 1081562ノート

反応式

HRID 1081562 の反応式
[NH2:1][C:2]1[C:3]([Br:12])=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[CH:7][CH:6]=[N:5]2.S(=O)(O)[O-].[Na+].[OH-].[Na+]>O>[BrH:12].[NH2:1][C:2]1[C:3]([Br:12])=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[CH:7][CH:6]=[N:5]2

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 149284425-Bromoquinoxalin-6-amine2 回HCID 23665763Sodium Bisulfite

生成物 1

HCID 183506656-Amino-5-bromoquinoxaline hydrobromide

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

The crude 6-amino-5-bromoquinoxaline from above was dissolved in water and saturated sodium bisulfite solution was added until the resulting solution tested negative with starch-iodide paper. The solution was then basified with 2N sodium hydroxide and extracted thoroughly with ethyl acetate. The organic extract was dried over magnesium sulfate and concentrated under reduced pressure to give the free base. The crude product was recrystallized from boiling benzene to give yellow crystals, m.p. 155°-6° C. Using various analytical procedures, the yellow crystals were determined to be 6-amino-5-bromoquinoxaline. The yield was 82%.

後処理

  1. extractionextracted thoroughly with ethyl acetate
  2. extractionThe organic extract
  3. dry with materialwas dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto give the free base
  6. customThe crude product was recrystallized
  7. customto give yellow crystals, m.p. 155°-6° C

出典と根拠

ORDレコード
ord-79ecfbceac11416eb0a083b626b59100
出典データセット
uspto-grants-1996_12
特許番号
US05587376

反応ノート

読み込み中…