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Hydrochloric Acid → 3-Bromo-2-benzoylamino-5-nitropyridine

HRID 256815
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HRID 256815 반응식
N1C=CC=CC=1.[NH2:7][C:8]1[C:13]([Br:14])=[CH:12][C:11]([N+:15]([O-:17])=[O:16])=[CH:10][N:9]=1.[C:18](Cl)(=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.Cl>C(#N)C>[Br:14][C:13]1[C:8]([NH:7][C:18](=[O:25])[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[N:9][CH:10]=[C:11]([N+:15]([O-:17])=[O:16])[CH:12]=1
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 7412Benzoyl chlorideHCID 27344122-Amino-3-bromo-5-nitropyridine

생성물 1

HCID 197840833-Bromo-2-benzoylamino-5-nitropyridine수율 89.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

20 mλ of pyridine was added to 2-amino-3-bromo-5-nitropyridine (A) (21.8 g; 0.1 mole) in 300 ,λ of acetonitrile at room temperature in a stream of nitrogen followed by addition of benzoylchloride (24.4 g; 0.2 mole) and agitation for 3 hours. Then dilute hydrochloric acid (0.1N) was added to the resulting mixture. After extraction with ethyl acetate, the resulting ethyl acetate solution was dried over anhydrous sodium sulfate. The solvent was distilled off under a reduced pressure. The residue was recrystallized from methanol to give 3-bromo-2-benzoylamino-5-nitropyridine (B) (28.7 g; 89%).

후처리

  1. extractionAfter extraction with ethyl acetate
  2. dry with materialthe resulting ethyl acetate solution was dried over anhydrous sodium sulfate
  3. distillationThe solvent was distilled off under a reduced pressure
  4. customThe residue was recrystallized from methanol

출처 및 근거

ORD 기록
ord-94847534671745609f1c58357504e4c3
출처 데이터셋
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05260177

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