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

HRID 40716노트

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HRID 40716 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-401742739efe4f8dbe8bad0c9f5cf879
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08530483B2

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