참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethanimidic acid, ethyl ester, hydrochloride (1:1) | HCID 2724290 | — |
| 반응물 | 5-(2-aminoethoxy)-7-chloro-1-[2-methoxy-4-(2-chlorobenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzoazepine | HCID 18917210 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | HCID 178493256 | HCID 178493256 | 69.8% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05622947 |
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| 출처 데이터셋 | uspto-grants-1997_04 |
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| ORD ID | ord-597fef2014da4af3ba5a26c8d03b5e73 |
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| 출처 메모 | uspto-grants-1997_04 |
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