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Sodium Hydroxide → 6-Amino-5-bromoquinoxaline hydrobromide

HRID 1081562
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HRID 1081562 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 149284425-Bromoquinoxalin-6-amine2회HCID 23665763Sodium Bisulfite

생성물 1

HCID 183506656-Amino-5-bromoquinoxaline hydrobromide

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-79ecfbceac11416eb0a083b626b59100
출처 데이터셋
uspto-grants-1996_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05587376

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