Hydrochloric Acid → HCID 57795472, Verbindung

HRID 1694517Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1694517
[CH3:1][N:2]1[C:6]2([CH2:15][CH2:14][C:9]3(OCC[O:10]3)[CH2:8][CH2:7]2)[CH2:5][N:4]([CH3:16])[C:3]1=[O:17].Cl>C1COCC1>[CH3:1][N:2]1[C:6]2([CH2:15][CH2:14][C:9](=[O:10])[CH2:8][CH2:7]2)[CH2:5][N:4]([CH3:16])[C:3]1=[O:17]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 57795511HCID 57795511, Verbindung

Produkt 1

HCID 57795472HCID 57795472, VerbindungAusbeute 66 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

1,3-Dimethyl-9,12-dioxa-1,3-diaza-dispiro[4.2.4.2]tetradecan-2-one (3.16 g, 13.2 mmol) was dissolved in 66 mL of THF and a portion of 130 mL of 3N HCl aqueous solution was added. The resulting mixture was stirred at 50° C. for two days. THF was removed under vacuum then the remaining mixture was extracted with two portions of dichloromethane. The organic portions were combined, dried over anhydrous Na2SO4 and concentrated. The crude was purified by silica gel column chromatography using a gradient from 2% CH2Cl2:MeOH to 10% CH2Cl2:MeOH as eluent to afford 1,3-dimethyl-1,3-diaza-spiro[4.5]decane-2,8-dione (1.7 g, 66%).

Aufarbeitung

  1. customTHF was removed under vacuum
  2. extractionthe remaining mixture was extracted with two portions of dichloromethane
  3. dry with materialdried over anhydrous Na2SO4
  4. concentrationconcentrated
  5. customThe crude was purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-79d853a1a7b8411cbd6c5a58abac4e09
Quelldatensatz
uspto-grants-2012_04
Patentnummer
US08158675B2

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