Pyridine → N-(2-hydroxy-5-nitrophenyl)butanamide

HRID 1886954

反応式

HRID 1886954 の反応式
[NH2:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[OH:11].N1C=CC=CC=1.[C:18](Cl)(=[O:22])[CH2:19][CH2:20][CH3:21]>ClCCl>[OH:11][C:3]1[CH:4]=[CH:5][C:6]([N+:8]([O-:10])=[O:9])=[CH:7][C:2]=1[NH:1][C:18](=[O:22])[CH2:19][CH2:20][CH3:21]

参加物

5

反応物 3

HCID 1049PyridineHCID 8855Butyryl chlorideHCID 36133892-Amino-4-Nitrophenol

生成物 1

HCID 3599768N-(2-hydroxy-5-nitrophenyl)butanamide収率 34%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-amino-4-nitrophenol (10 g, 64.9 mmol) in dichloromethane (250 mL) under nitrogen at 0° C. was added pyridine (10.5 mL, 129.9 mmol) followed by butyryl chloride (7.05 mL, 68.2 mmol) over a period of 5 min. After 30 min at 0° C., the solution was left warming up to room temperature for 2 days. The organic layer was washed with aqueous copper sulfate solution and brine. Insoluble material from the aqueous layer was filtered off and washed with water to afford 4.95 g (34%) of the title compound.

後処理

  1. waitthe solution was left
  2. washThe organic layer was washed with aqueous copper sulfate solution and brine
  3. filtrationInsoluble material from the aqueous layer was filtered off
  4. washwashed with water

出典と根拠

ORDレコード
ord-ec65866deaea4f778d6801b4cbdddc5a
出典データセット
uspto-grants-2013_08
特許番号
US08501713B2

関連ノート

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