Sodium Hydroxide → 8-(4-Methyl-3-oxo-piperazin-1-yl)-1,4-dioxa-spiro[4,5]decane

HRID 1672133Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1672133
C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[CH3:15][N:16]1[CH2:21][CH2:20][NH:19][CH2:18][C:17]1=[O:22].[O:23]1[C:27]2([CH2:32][CH2:31][C:30](=O)[CH2:29][CH2:28]2)[O:26][CH2:25][CH2:24]1.[OH-].[Na+]>ClCCl.C(O)(=O)C>[CH3:15][N:16]1[CH2:21][CH2:20][N:19]([CH:30]2[CH2:31][CH2:32][C:27]3([O:26][CH2:25][CH2:24][O:23]3)[CH2:28][CH2:29]2)[CH2:18][C:17]1=[O:22]

Komponenten

7

Edukt 4

HCID 14798Sodium HydroxideHCID 5674151,4-Dioxaspiro[4.5]decan-8-oneHCID 43990421-Methylpiperazin-2-oneHCID 5049666Sodium triacetoxyborohydride

Produkt 1

HCID 591581918-(4-Methyl-3-oxo-piperazin-1-yl)-1,4-dioxa-spiro[4,5]decane

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittelHCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

26.18 g Sodium triacetoxyborohydride are added at 5° C. to a solution of 10.0 g 4-methyl-3-oxo-piperazine, 13.51 g 1,4-dioxa-spiro[4,5]decan-8-one, 5.65 ml acetic acid and 200 ml dichloromethane. After 23 hours stirring at ambient temperature 100 ml dichloromethane and 100 ml 4N sodium hydroxide solution are added. The phases are separated and the organic phase is evaporated down. The residue is purified by chromatography.

Aufarbeitung

  1. additionare added
  2. customThe phases are separated
  3. customthe organic phase is evaporated down
  4. customThe residue is purified by chromatography

Quellen und Nachweise

ORD-Eintrag
ord-a4429f6a75464374901cdeafce5ea91b
Quelldatensatz
uspto-grants-2011_08
Patentnummer
US07998949B2

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