Ethanimidic acid, ethyl ester, hydrochloride (1:1) → HCID 178493256, 화합물

HRID 1291555

반응식

HRID 1291555 반응식
Cl.[C:2](=[NH:7])(OCC)[CH3:3].[NH2:8][CH2:9][CH2:10][O:11][CH:12]1[C:18]2[CH:19]=[C:20]([Cl:23])[CH:21]=[CH:22][C:17]=2[N:16]([C:24](=[O:43])[C:25]2[CH:30]=[CH:29][C:28]([NH:31][C:32](=[O:40])[C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][C:34]=3[Cl:39])=[CH:27][C:26]=2[O:41][CH3:42])[CH2:15][CH2:14][CH2:13]1>C(O)C>[ClH:23].[NH:7]=[C:2]([NH:8][CH2:9][CH2:10][O:11][CH:12]1[C:18]2[CH:19]=[C:20]([Cl:23])[CH:21]=[CH:22][C:17]=2[N:16]([C:24](=[O:43])[C:25]2[CH:30]=[CH:29][C:28]([NH:31][C:32](=[O:40])[C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][C:34]=3[Cl:39])=[CH:27][C:26]=2[O:41][CH3:42])[CH2:15][CH2:14][CH2:13]1)[CH3:3]

참가 물질

4

반응물 2

HCID 2724290Ethanimidic acid, ethyl ester, hydrochloride (1:1)2회HCID 189172105-(2-aminoethoxy)-7-chloro-1-[2-methoxy-4-(2-chlorobenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzoazepine

생성물 1

HCID 178493256HCID 178493256, 화합물수율 69.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

0.129 g of ethyl acetoimidate hydrochloride was added to 15 ml of a suspension of 0.5 g of 5-(2-amino-ethoxy)-7-chloro-1-[2-methoxy-4-(2-chlorobenzoylamino)-benzoyl]-2,3,4,5-tetrahydro-1H-benzoazepine in ethanol with ice-cooling. The mixture was stirred overnight at room temperature. Then, 0.163 g of ethyl acetoimidate hydrochloride was further added. The mixture was stirred at 50° C. for 7 hours and then refluxed for 3 hours. After cooling, the reaction mixture was subjected to filtration to remove insolubles. The filtrate was concentrated. The residue was purified by silica gel column chromatography (elutant: dichloromethane/methanol=30/1) to obtain 0.2 g of 5-[2-(1-iminoethyl)aminoethoxy]-7-chloro-1-[2-methoxy-4-(2-chlorobenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzo-azepine hydrochloride.

후처리

  1. temperaturecooling
  2. stirringThe mixture was stirred at 50° C. for 7 hours
  3. temperaturerefluxed for 3 hours
  4. temperatureAfter cooling
  5. filtrationthe reaction mixture was subjected to filtration
  6. customto remove insolubles
  7. concentrationThe filtrate was concentrated
  8. customThe residue was purified by silica gel column chromatography (elutant: dichloromethane/methanol=30/1)

출처 및 근거

ORD 기록
ord-44b1aaefbd284fb89ff9e32a67de9e7b
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05753644

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