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

HRID 256815
ノート
印刷プレビュー

反応式

HRID 256815 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 197840833-Bromo-2-benzoylamino-5-nitropyridine収率 89.1%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-94847534671745609f1c58357504e4c3
出典データセット
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05260177

反応ノート

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