Sodium Iodide → HCID 18917235、化合物

HRID 1291553ノート

反応式

HRID 1291553 の反応式
C1(C)C=CC(S(O[CH2:11][CH2:12][O:13][CH:14]2[C:20]3[CH:21]=[C:22]([F:25])[CH:23]=[CH:24][C:19]=3[N:18]([C:26](=[O:45])[C:27]3[CH:32]=[CH:31][C:30]([NH:33][C:34](=[O:42])[C:35]4[CH:40]=[CH:39][CH:38]=[CH:37][C:36]=4[CH3:41])=[CH:29][C:28]=3[O:43][CH3:44])[CH2:17][CH2:16][CH2:15]2)(=O)=O)=CC=1.[CH3:47][N:48]1[CH2:53][CH2:52][NH:51][CH2:50][CH2:49]1.[I-].[Na+]>CN(C)C=O>[CH3:47][N:48]1[CH2:53][CH2:52][N:51]([CH2:11][CH2:12][O:13][CH:14]2[C:20]3[CH:21]=[C:22]([F:25])[CH:23]=[CH:24][C:19]=3[N:18]([C:26](=[O:45])[C:27]3[CH:32]=[CH:31][C:30]([NH:33][C:34](=[O:42])[C:35]4[CH:40]=[CH:39][CH:38]=[CH:37][C:36]=4[CH3:41])=[CH:29][C:28]=3[O:43][CH3:44])[CH2:17][CH2:16][CH2:15]2)[CH2:50][CH2:49]1

参加物

5

反応物 3

HCID 5238Sodium IodideHCID 531671-MethylpiperazineHCID 189171765-[2-(p-Toluenesulfonyloxy)ethoxy]-7-fluoro-1-[2-methoxy-4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine

生成物 1

HCID 18917235HCID 18917235、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

In 10 ml of dimethylformamide were dispersed 0.4 g of 5-[2-(p-toluenesulfonyloxy)ethoxy]-7-fluoro-1-[2-methoxy-4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzoazepine, 0.38 ml of N-methylpiperazine and 0.3 g of sodium iodide. The dispersion was stirred at room temperature for 3 days. The reaction mixture was concentrated. The residue was mixed with water and the mixture was subjected to extraction with ethyl acetate. The extract was dried over sodium carbonate and purified by silica gel column chromatography (elutant: dichloromethane/-methanol=10/1) to obtain 1.15 g of 5-[2-(4-methyl-1-piperazinyl)ethoxy]-7-fluoro-1-[2-methoxy-4-(2-methyl-benzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzoazepine. Colorless and amorphous

後処理

  1. concentrationThe reaction mixture was concentrated
  2. additionThe residue was mixed with water
  3. extractionthe mixture was subjected to extraction with ethyl acetate
  4. dry with materialThe extract was dried over sodium carbonate
  5. custompurified by silica gel column chromatography (elutant: dichloromethane/-methanol=10/1)

出典と根拠

ORDレコード
ord-8873173aa6ec49b0b5c5b0a7b06292d3
出典データセット
uspto-grants-1998_05
特許番号
US05753644

反応ノート

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