Hydrochloric Acid → Dimethylamino-(1,4-dioxaspiro[4.5]dec-8-yl)-acetonitrile

HRID 12641Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 12641
[CH3:1][NH:2][CH3:3].[O:4]1[C:8]2([CH2:13][CH2:12][CH:11]([CH:14]=O)[CH2:10][CH2:9]2)[O:7][CH2:6][CH2:5]1.[C-:16]#[N:17].[K+].Cl>O.CO>[CH3:1][N:2]([CH:14]([CH:11]1[CH2:10][CH2:9][C:8]2([O:4][CH2:5][CH2:6][O:7]2)[CH2:13][CH2:12]1)[C:16]#[N:17])[CH3:3]

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 674DimethylamineHCID 9032Potassium CyanideHCID 98989471,4-Dioxaspiro(4.5)decane-8-carbaldehyde

Produkt 1

HCID 57839521Dimethylamino-(1,4-dioxaspiro[4.5]dec-8-yl)-acetonitrile

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

40% aqueous dimethylamine solution (85 ml, 0.67 mole), 1,4-dioxa-spiro-[4.5]decane-8-carbaldehyde 5 (240 g, 0.141 mole) and potassium cyanide (22.05 g, 0.338 mole) were added while cooling with ice to a mixture of 4N hydrochloric acid (37 ml) and methanol (22 ml). The mixture was stirred for four days at room temperature and then, after adding water (80 ml), extracted with diethyl ether (4×100 ml). The organic phase was dried over sodium sulfate, concentrated by evaporation in vacuo, and the product was obtained as a white solid.

Aufarbeitung

  1. extractionextracted with diethyl ether (4×100 ml)
  2. dry with materialThe organic phase was dried over sodium sulfate
  3. concentrationconcentrated by evaporation in vacuo
  4. customthe product was obtained as a white solid

Quellen und Nachweise

ORD-Eintrag
ord-85f0a1c8da154ceeb53790dd29fb205d
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07728028B2

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