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Sodium Bicarbonate → 4-[5-(4-Chlorophenyl)-2-thiophenesulfonyl]-1-[1-(4-pyridyl)piperidin-4-ylmethyl]-2-piperazinone

HRID 2186164
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2186164
Cl.[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[S:13][C:12]([S:14]([N:17]3[CH2:22][CH2:21][N:20]([CH2:23][CH:24]4[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]4)[C:19](=[O:30])[CH2:18]3)(=[O:16])=[O:15])=[CH:11][CH:10]=2)=[CH:5][CH:4]=1.Cl.Cl[C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][N:34]=1.C(=O)(O)[O-].[Na+]>>[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[S:13][C:12]([S:14]([N:17]3[CH2:22][CH2:21][N:20]([CH2:23][CH:24]4[CH2:29][CH2:28][N:27]([C:37]5[CH:36]=[CH:35][N:34]=[CH:33][CH:38]=5)[CH2:26][CH2:25]4)[C:19](=[O:30])[CH2:18]3)(=[O:16])=[O:15])=[CH:11][CH:10]=2)=[CH:5][CH:4]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 3

HCID 516892Sodium BicarbonateHCID 156199202-Chloropyridine--hydrogen chloride (1/1)HCID 234473094-[5-(4-Chlorophenyl)-2-thiophenesulfonyl]-1-(piperidin-4-ylmethyl)-2-piperazinone hydrochloride

Produkt 1

HCID 234474724-[5-(4-Chlorophenyl)-2-thiophenesulfonyl]-1-[1-(4-pyridyl)piperidin-4-ylmethyl]-2-piperazinone

Reaktionsbedingungen

Temperatur
130 °C

Versuchsvorschrift

To 1-[1-(tert-butoxycarbonyl)piperidin-4-ylmethyl]-4-[5-(4-chlorophenyl)-2-thiophenesulfonyl]-2-piperazinone (115 mg) were added 4N hydrochloric acid in ethyl acetate (10 ml) and methanol (4 ml), and the mixture was stirred at room temperature for 30 minutes. The reaction solution was concentrated to give crude crystals of 4-[5-(4-chlorophenyl)-2-thiophenesulfonyl]-1-(piperidin-4-ylmethyl)-2-piperazinone hydrochloride. A mixture of the obtained 4-[5-(4-chlorophenyl)-2-thiophenesulfonyl]-1-(piperidin-4-ylmethyl)-2-piperazinone hydrochloride and chloropyridine hydrochloride (85 mg) was added to sodium bicarbonate solution, and the mixture was extracted with dichloromethane (twice), dried and concentrated. To the residue was added isoamylalcohol (10 ml), and the mixture was stirred at 130° C. for 15 hours. The reaction solution was concentrated, and the residue was dissolved in dichloromethane. The solution was washed with 1N sodium hydroxide solution, dried and concentrated, and the residue was purified with silica gel column chromatography (dichloromethane:methanol containing 10% ammonia solution=10:1) to give colorless solid of the title compound (42 mg).

Aufarbeitung

  1. extractionthe mixture was extracted with dichloromethane (twice),
  2. customdried
  3. concentrationconcentrated
  4. additionTo the residue was added isoamylalcohol (10 ml)
  5. concentrationThe reaction solution was concentrated
  6. dissolutionthe residue was dissolved in dichloromethane
  7. washThe solution was washed with 1N sodium hydroxide solution
  8. customdried
  9. concentrationconcentrated
  10. customthe residue was purified with silica gel column chromatography (dichloromethane:methanol containing 10% ammonia solution=10:1)

Quellen und Nachweise

ORD-Eintrag
ord-b71c4b1bff904759862c43a98430d54c
Quelldatensatz
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06403595B1

Notizen zur Reaktion

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