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

HRID 1247136

반응식

HRID 1247136 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fb969452a7824d4d87b294b4c0670fec
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07129245B2

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