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

HRID 991421ノート

反応式

HRID 991421 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
115 °C

実験手順

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.;

後処理

  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

出典と根拠

ORDレコード
ord-b44995c9e70244ae9b866686a38d709f
出典データセット
uspto-grants-2002_10
特許番号
US06465455B1

反応ノート

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