Sodium Iodide → HCID 18917235, 화합물

HRID 5589노트

반응식

HRID 5589 반응식
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

참가 물질

5

반응물 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

생성물 1

HCID 18917235HCID 18917235, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

5-[2-(p-Toluenesulfonyloxy)ethoxy]-7-fluoro-1-[2-methoxy-4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.4 g), N-methylpiperazine (0.38 ml) and sodium iodide (0.3 g) are dispersed in dimethylformamide (10 ml), and the mixture is stirred at room temperature for 3 days. The reaction mixture is concentrated, and thereto is added water. The mixture is extracted with ethyl acetate, and the extract is dried over sodium carbonate, and purified by silica gel column chromatography (eluent; dichloromethane:methanol=10:1) to give 5-[2-(4-methyl-1-piperazinyl)-ethoxy]-7-fluoro-1-[2-methoxy-4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.15 g) as colorless amorphous.

후처리

  1. concentrationThe reaction mixture is concentrated
  2. additionis added water
  3. extractionThe mixture is extracted with ethyl acetate
  4. dry with materialthe extract is dried over sodium carbonate
  5. custompurified by silica gel column chromatography (eluent; dichloromethane:methanol=10:1)

출처 및 근거

ORD 기록
ord-09459eb81e7b4be98bb3082439814f71
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05244898

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