Triethylamine → HCID 10143653, Verbindung

HRID 2214827Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2214827
C(N(CC)CC)C.Cl.[CH2:9]([O:11][C:12]([NH:14][C:15]1([CH2:28][N:29]2[CH2:34][CH2:33][NH:32][CH2:31][C:30]2=[O:35])[CH2:20][CH2:19][N:18]([C:21]2[CH:26]=[CH:25][N:24]=[C:23]([CH3:27])[CH:22]=2)[CH2:17][CH2:16]1)=[O:13])[CH3:10].[CH:36]([C:38]1[CH:43]=[CH:42][C:41]([S:44](Cl)(=[O:46])=[O:45])=[CH:40][CH:39]=1)=[CH2:37].C(=O)([O-])[O-].[Na+].[Na+]>ClCCl>[CH2:9]([O:11][C:12]([NH:14][C:15]1([CH2:28][N:29]2[CH2:34][CH2:33][N:32]([S:44]([C:41]3[CH:42]=[CH:43][C:38]([CH:36]=[CH2:37])=[CH:39][CH:40]=3)(=[O:46])=[O:45])[CH2:31][C:30]2=[O:35])[CH2:16][CH2:17][N:18]([C:21]2[CH:26]=[CH:25][N:24]=[C:23]([CH3:27])[CH:22]=2)[CH2:19][CH2:20]1)=[O:13])[CH3:10]

Komponenten

6

Edukt 4

HCID 8471TriethylamineHCID 10340Sodium CarbonateHCID 9855777Styrene-4-sulfonyl chlorideHCID 219483121-{[4-Ethoxycarbonylamino-1-(2-methyl-4-pyridyl)-4-piperidinyl]methyl}-2-piperazinone Hydrochloride

Produkt 1

HCID 10143653HCID 10143653, VerbindungAusbeute 45,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Triethylamine (260 mg) was added to a solution of 1-{[4-ethoxycarbonylamino-1-(2-methyl-4-pyridyl)-4-piperidinyl]methyl}-2-piperazinone hydrochloride (263 mg) in dichloromethane (20 ml), 4-vinylbenzenesulfonyl chloride (194 mg) was added at 0° C., and the mixture was stirred at room temperature for 1 hour. To the reaction solution was added an aqueous sodium carbonate solution, the material was extracted with dichloromethane, dried, concentrated, purified by column chromatography (dichloromethane:10% aqueous ammonia-containing methanol=20:1), and crystallized from diisopropyl ether to obtain the colorless crystalline title compound (157 mg).

Aufarbeitung

  1. additionwas added at 0° C.
  2. extractionthe material was extracted with dichloromethane
  3. customdried
  4. concentrationconcentrated
  5. custompurified by column chromatography (dichloromethane:10% aqueous ammonia-containing methanol=20:1)
  6. customcrystallized from diisopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-914417d199e34fb19a8c3d22559b993e
Quelldatensatz
uspto-grants-2006_09
Patentnummer
US07109200B2

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