Ethanol → 6-{4-[3-(4-Chlorobenzoyl)-3-hydroxyliminopropyl]-1-piperazinylcarbonyl}-3,4-dihydrocarbostyril

HRID 1460680ノート

反応式

HRID 1460680 の反応式
ClC1C=CC(C(CC[C:10]2([C:21]([N:23]3[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]3)=[O:22])[CH2:19][C:18]3[C:13](=[CH:14][CH:15]=C[CH:17]=3)[NH:12]C2=O)=O)=CC=1.[ClH:31].[NH2:32][OH:33].[C:34]([O-:37])(=O)[CH3:35].[Na+].[CH2:39]([OH:41])[CH3:40]>O>[Cl:31][C:13]1[CH:18]=[CH:17][C:40]([C:39]([C:19](=[N:32][OH:33])[CH2:10][CH2:21][N:26]2[CH2:25][CH2:24][N:23]([C:21]([C:10]3[CH:19]=[C:18]4[C:13](=[CH:14][CH:15]=3)[NH:12][C:34](=[O:37])[CH2:35][CH2:17]4)=[O:22])[CH2:28][CH2:27]2)=[O:41])=[CH:15][CH:14]=1

参加物

6

反応物 4

HCID 702EthanolHCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 1317170952-(4-Chlorobenzoyl)ethyl[-1-piperazinylcarbonyl}-3,4-dihydrocarbostyril

生成物 1

HCID 881243866-{4-[3-(4-Chlorobenzoyl)-3-hydroxyliminopropyl]-1-piperazinylcarbonyl}-3,4-dihydrocarbostyril

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

1.7 Grams of 6-{4-[2-(4-chlorobenzoyl)ethyl[-1-piperazinylcarbonyl}-3,4-dihydrocarbostyril, 0.83 g of hydroxylamine hydrochloride and 2.29 g of sodium acetate were dissolved in 40 ml of ethanol and 20 ml of water, and the solution was stirred overnight at room temperature. Then the reaction mixture was concentrated under reduced pressure, then the residue thus obtained was extracted with chloroform, the extract was dried with anhydrous sodium carbonate, then the solvent was removed by evaporation. The residue thus obtained was purified by means of a silica gel column chromatography (eluent: dichloromethane:methanol =50:1), then recrystallized from ethanol to yield 1.2 g of 6-{4[-3-(4-chlorobenzoyl)-3-hydroxyliminopropyl]-1-piperazinylcarbonyl}-3,4-dihydrocarbostyril. White powdery substance. Melting point: 207° C.-209° C. (decomp.).

後処理

  1. concentrationThen the reaction mixture was concentrated under reduced pressure
  2. customthe residue thus obtained
  3. extractionwas extracted with chloroform
  4. dry with materialthe extract was dried with anhydrous sodium carbonate
  5. customthe solvent was removed by evaporation
  6. customThe residue thus obtained
  7. customwas purified by means of a silica gel column chromatography (eluent: dichloromethane:methanol =50:1)
  8. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-8cf757d0714b4a5aa2e8e9b21c6197bc
出典データセット
uspto-grants-1991_12
特許番号
US05071856

反応ノート

読み込み中…