Pyridine → N-(5-chloropyridin-2-yl)-2-nitrobenzamide

HRID 1247136

反応式

HRID 1247136 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][N:3]=1.N1C=CC=CC=1.[N+:15]([C:18]1[CH:26]=[CH:25][CH:24]=[CH:23][C:19]=1[C:20](Cl)=[O:21])([O-:17])=[O:16]>ClCCl>[Cl:8][C:5]1[CH:6]=[CH:7][C:2]([NH:1][C:20](=[O:21])[C:19]2[CH:23]=[CH:24][CH:25]=[CH:26][C:18]=2[N+:15]([O-:17])=[O:16])=[N:3][CH:4]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 118752-Nitrobenzoyl chlorideHCID 661742-Amino-5-chloropyridine

生成物 1

HCID 766647N-(5-chloropyridin-2-yl)-2-nitrobenzamide収率 79.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirring solution of 2-amino-5-chloropyridine (3.7 g, 29 mmol) and pyridine (7.3 mL, 90 mmol) in dichloromethane was added 2-nitrobenzoyl chloride (5.7 g, 30 mmol). After stirring for 4 h, the solvents were removed in vacuo and the residue partitioned between ethyl acetate and water. The organic phase was washed with brine, dried over magnesium sulfate, filtered, and concentrated in vacuo. After standing at room temperature overnight, the mixture was filtered to give 6.4 g (79%) of a white solid.

後処理

  1. customthe solvents were removed in vacuo
  2. customthe residue partitioned between ethyl acetate and water
  3. washThe organic phase was washed with brine
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. waitAfter standing at room temperature overnight
  8. filtrationthe mixture was filtered

出典と根拠

ORDレコード
ord-fb969452a7824d4d87b294b4c0670fec
出典データセット
uspto-grants-2006_10
特許番号
US07129245B2

関連ノート

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