Water → N-[2-chloro-5-(3-morpholinobenzamido)phenyl]-3,4-dimethoxybenzamide

HRID 991421노트

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HRID 991421 반응식
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[CH:8]=[C:9]([CH:13]=[CH:14][CH:15]=2)[C:10](Cl)=[O:11])[CH2:3][CH2:2]1.[NH2:16][C:17]1[CH:18]=[CH:19][C:20]([Cl:36])=[C:21]([NH:23][C:24](=[O:35])[C:25]2[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[C:27]([O:33][CH3:34])[CH:26]=2)[CH:22]=1.O>N1C=CC=CC=1>[Cl:36][C:20]1[CH:19]=[CH:18][C:17]([NH:16][C:10](=[O:11])[C:9]2[CH:13]=[CH:14][CH:15]=[C:7]([N:4]3[CH2:5][CH2:6][O:1][CH2:2][CH2:3]3)[CH:8]=2)=[CH:22][C:21]=1[NH:23][C:24](=[O:35])[C:25]1[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[C:27]([O:33][CH3:34])[CH:26]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 18413853N-(5-amino-2-chlorophenyl)-3,4-dimethoxybenzamideHCID 220579723-Morpholinobenzoyl chloride

생성물 1

HCID 9913728N-[2-chloro-5-(3-morpholinobenzamido)phenyl]-3,4-dimethoxybenzamide수율 36.4%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
115 °C

실험 절차

3-Morpholinobenzoyl chloride (0.15 g) was added to a stirred solution of N-(5-amino-2-chlorophenyl)-3,4-dimethoxybenzamide (0.17 g) in pyridine (3 ml). The reaction mixture was stirred and heated to 115° C. for 18 hours. The mixture was allowed to cool and poured into water. The mixture was extracted with methylene chloride. The organic extract was dried (MgSO4) and evaporated. The resultant solid was azeotroped with toluene and triturated under diethyl ether to give the title compound (0.1 g), m.p. 147.9-148.3° C.;

후처리

  1. temperatureto cool
  2. extractionThe mixture was extracted with methylene chloride
  3. extractionThe organic extract
  4. dry with materialwas dried (MgSO4)
  5. customevaporated
  6. customThe resultant solid was azeotroped with toluene
  7. customtriturated under diethyl ether

출처 및 근거

ORD 기록
ord-b44995c9e70244ae9b866686a38d709f
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06465455B1

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