Hydrogen Bromide → 6-Bromo-3-nitro-2-pyridinamine

HRID 1072791노트

반응식

HRID 1072791 반응식
[BrH:1].[NH2:2][C:3]1[C:8]([N+:9]([O-:11])=[O:10])=[CH:7][CH:6]=[C:5](Cl)[N:4]=1>C(O)(=O)C>[NH2:2][C:3]1[C:8]([N+:9]([O-:11])=[O:10])=[CH:7][CH:6]=[C:5]([Br:1])[N:4]=1

참가 물질

4

반응물 2

HCID 260Hydrogen Bromide2회HCID 27240356-Chloro-3-nitropyridin-2-ylamine

생성물 1

HCID 120977456-Bromo-3-nitro-2-pyridinamine

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

반응 조건

온도
100 °C

실험 절차

A 30% solution of hydrogen bromide in acetic acid (10 ml) was added to 2-amino-6-chloro-3-nitropyridine (1.0 g) at room temperature and the mixture was heated at 100° C. After 24 hr, a 30% solution of hydrogen bromide in acetic acid (5 ml) was added. After 48 hr, the reaction mixture was cooled and concentrated. The residue was neutralized with 28% aqueous ammonia and extracted three times with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, filtered and concentrated. The residue was crystallized from isopropyl ether to give the objective compound (1.14 g) as yellow crystals.

후처리

  1. waitAfter 48 hr
  2. temperaturethe reaction mixture was cooled
  3. concentrationconcentrated
  4. extractionextracted three times with ethyl acetate
  5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe residue was crystallized from isopropyl ether

출처 및 근거

ORD 기록
ord-4bd694c7b0a84d14bc5a8ab1317d6890
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06911469B2

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