Ethanimidic acid, ethyl ester, hydrochloride (1:1) → HCID 178493256、化合物

HRID 54755

反応式

HRID 54755 の反応式
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]

参加物

4

反応物 2

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

生成物 1

HCID 178493256HCID 178493256、化合物収率 69.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-597fef2014da4af3ba5a26c8d03b5e73
出典データセット
uspto-grants-1997_04
特許番号
US05622947

関連ノート

読み込み中…