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Ammonia → {(3S)-3-(3,4-Dichlorophenyl)-1-[6-(dimethylamino)-2-pyridinyl]-6-oxopiperidinyl}acetaldehyde Hydrochloride

HRID 1829174
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1829174
[C:1](=[O:4])([O-])[O-].[K+].[K+].Br[C:8]1[N:13]=[C:12]([N:14]([CH3:16])[CH3:15])[CH:11]=[CH:10][CH:9]=1.[Cl:17][C:18]1[CH:19]=[C:20]([C@:25]2([CH2:32][CH:33]3OCCO3)CN[C:28](=[O:31])[CH2:27][CH2:26]2)[CH:21]=[CH:22][C:23]=1[Cl:24].[ClH:38].[NH3:39]>CN1CCCC1=O.[Cu]I>[ClH:17].[Cl:38][C:22]1[CH:21]=[C:20]([C@@H:25]2[CH2:26][CH2:27][C:28](=[O:31])[N:39]([C:8]3[CH:9]=[CH:10][CH:11]=[C:12]([N:14]([CH3:16])[CH3:15])[N:13]=3)[CH:32]2[CH2:33][CH:1]=[O:4])[CH:19]=[CH:18][C:23]=1[Cl:24]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 10882069(5S)-5-(3,4-dichlorophenyl)-5-(1,3-dioxolan-2-ylmethyl)-2-piperidinoneHCID 140060626-bromo-N,N-dimethylpyridin-2-amine

Produkt 1

HCID 86593350
{(3S)-3-(3,4-Dichlorophenyl)-1-[6-(dimethylamino)-2-pyridinyl]-6-oxopiperidinyl}acetaldehyde Hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)KatalysatorHCID 13387N-methyl-2-pyrrolidoneLösungsmittel

Reaktionsbedingungen

Temperatur
140 °C

Versuchsvorschrift

Copper (I) iodide (6.4 g, 33.3 mmol), potassium carbonate (6.3 g, 45.4 mmol) and 6-bromo-2-(dimethylamino)pyridine (WO 9843971) (9 g, 45.4 mmol) were added consecutively to a solution of (5S)-5-(3,4-dichlorophenyl)-5-(1,3-dioxolan-2-ylmethyl)-2-piperidinone (WO 9807722) (10 g, 30.3 mmol), in 1-methyl-2-pyrrolidinone (50 ml), and the mixture was stirred at 140° C. for 4 hours. The cooled mixture was poured into 4N hydrochloric acid, then carefully basified using 10% aqueous ammonia. The aqueous mixture was extracted with ethyl acetate (3×200 ml), and the combined organic extracts were washed with brine, dried (MgSO4) and evaporated under reduced pressure to give an orange oil. The crude product was purified by column chromatography on silica gel using methanol:dichloromethane (5:95) as eluant, and repeated using ethyl acetate as eluant. The product was treated with 1N ethereal hydrochloric acid, and evaporated under reduced pressure to afford the title compound.

Aufarbeitung

  1. extractionThe aqueous mixture was extracted with ethyl acetate (3×200 ml)
  2. washthe combined organic extracts were washed with brine
  3. dry with materialdried (MgSO4)
  4. customevaporated under reduced pressure
  5. customto give an orange oil
  6. customThe crude product was purified by column chromatography on silica gel
  7. additionThe product was treated with 1N ethereal hydrochloric acid
  8. customevaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-21c838b827c04abdbed331dd02a294dc
Quelldatensatz
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07060836B2

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