Sodium Carbonate → 1-{N-{3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]-propyl}-N-methylaminoacetyl}-4-phenoxypiperidine

HRID 463310Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 463310
Cl.CO.C(O)(=O)C(O)=O.[F:10][C:11]1[CH:16]=[CH:15][C:14]([C:17]2([CH2:22][CH2:23][CH2:24][N:25]([CH2:27][C:28]([N:30]3[CH2:35][CH2:34][CH:33]([O:36][C:37]4[CH:42]=[CH:41][CH:40]=[C:39](Cl)[CH:38]=4)[CH2:32][CH2:31]3)=[O:29])[CH3:26])[O:21][CH2:20][CH2:19][O:18]2)=[CH:13][CH:12]=1.[H][H].C(=O)([O-])[O-].[Na+].[Na+]>[Pd].CO>[F:10][C:11]1[CH:16]=[CH:15][C:14]([C:17]2([CH2:22][CH2:23][CH2:24][N:25]([CH2:27][C:28]([N:30]3[CH2:31][CH2:32][CH:33]([O:36][C:37]4[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=4)[CH2:34][CH2:35]3)=[O:29])[CH3:26])[O:18][CH2:19][CH2:20][O:21]2)=[CH:13][CH:12]=1

Komponenten

7

Edukt 4

HCID 10340Sodium CarbonateHCID 202831291-{N-{3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]propyl}-N-methylaminoacetyl}-4-(3-chlorophenoxy)piperidine oxalateHCID 21893726Hydrochloride methanolHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 202831171-{N-{3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]-propyl}-N-methylaminoacetyl}-4-phenoxypiperidine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

A suspension prepared from 2.25 g of 5% palladium on carbon, 400 ml of methanol, 0.2 ml of saturated HCl/methanol and 11.19 g (19.3 mmol) of 1-{N-{3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]propyl}-N-methylaminoacetyl}-4-(3-chlorophenoxy)piperidine oxalate was shaken under 50 psi hydrogen at 50° for 4 hours. The mixture was allowed to cool to room temperature and filtered, and the solvent was evaporated to provide an oil. The oil was shaken with saturated sodium carbonate, extracted with ether, dried over potassium carbonate, filtered, and the solvent evaporated to provide 1-{N-{3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]-propyl}-N-methylaminoacetyl}-4-phenoxypiperidine.

Aufarbeitung

  1. filtrationfiltered
  2. customthe solvent was evaporated
  3. customto provide an oil
  4. extractionextracted with ether
  5. dry with materialdried over potassium carbonate
  6. filtrationfiltered
  7. customthe solvent evaporated

Quellen und Nachweise

ORD-Eintrag
ord-51b17dd9911a4565b4e424e5ac0c3315
Quelldatensatz
uspto-grants-1985_05
Patentnummer
US04518713

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