Water → N-(2,6-dichloro-pyridin-3-yl)-4-methoxy-benzamide

HRID 40716ノート

反応式

HRID 40716 の反応式
[CH3:1][O:2][C:3]1[CH:11]=[CH:10][C:6]([C:7](Cl)=[O:8])=[CH:5][CH:4]=1.[Cl:12][C:13]1[C:18]([NH2:19])=[CH:17][CH:16]=[C:15]([Cl:20])[N:14]=1.O>N1C=CC=CC=1>[Cl:12][C:13]1[C:18]([NH:19][C:7](=[O:8])[C:6]2[CH:10]=[CH:11][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)=[CH:17][CH:16]=[C:15]([Cl:20])[N:14]=1

参加物

5

反応物 3

HCID 962WaterHCID 7477p-Anisoyl chlorideHCID 1128462,6-Dichloro-3-pyridylamine

生成物 1

HCID 58220150N-(2,6-dichloro-pyridin-3-yl)-4-methoxy-benzamide収率 95%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
0 °C

実験手順

4-Methoxy-benzoyl chloride (4.15 mL, 30.7 mmol) was added dropwise to a stirred, cooled 0° C. mixture of 2,6-dichloro-pyridin-3-ylamine (5 g, 30.7 mmol) in pyridine (31 mL). Following addition, the reaction mixture was allowed to warm to room temperature and stirring was continued for 30 minutes, at which point the reaction mixture was poured into water causing the formation of a precipitate which was collected by filtration. The collected solids were washed with additional water before drying overnight in vacuo affording N-(2,6-dichloro-pyridin-3-yl)-4-methoxy-benzamide (8.66 g, 29.1 mmol, 95% yield) which was used in subsequent reactions without further purification. ES MS (M+H+)=297.

後処理

  1. additionaddition
  2. temperatureto warm to room temperature
  3. filtrationwas collected by filtration
  4. washThe collected solids were washed with additional water
  5. custombefore drying overnight in vacuo

出典と根拠

ORDレコード
ord-401742739efe4f8dbe8bad0c9f5cf879
出典データセット
uspto-grants-2013_09
特許番号
US08530483B2

反応ノート

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