Dimethylformamide dimethyl acetal → 1-Penten-3-one, 1-(dimethylamino)-4,4-dimethoxy-

HRID 1181558Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1181558
[CH3:1][O:2][C:3]([O:8][CH3:9])([CH3:7])[C:4](=[O:6])[CH3:5].CO[CH:12](OC)[N:13]([CH3:15])[CH3:14]>CO>[CH3:12][N:13]([CH3:15])[CH:14]=[CH:5][C:4](=[O:6])[C:3]([O:8][CH3:9])([O:2][CH3:1])[CH3:7]

Komponenten

4

Edukt 2

HCID 78373Dimethylformamide dimethyl acetalHCID 1408713,3-Dimethoxy-2-butanone

Produkt 1

HCID 5668111-Penten-3-one, 1-(dimethylamino)-4,4-dimethoxy-Ausbeute 90,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

100 g (0.76 mol) of 3,3-dimethoxy-2-butanone (16) were stirred together with 90.2 g of N,N-dimethylformamide dimethyl acetal (17) (0.76 mol) at 120° C. for 48 h. The methanol which was formed in the reaction was removed continuously from the reaction solution by means of distillation. Crystallization occurred spontaneously when the solution was cooled, with the crystallization being brought to completion by adding a little heptane. This resulted in 128.24 g of crude product 18 (yield 90%), which was reacted without any further purification.

Aufarbeitung

  1. customwas removed continuously from the reaction solution by means of distillation
  2. customCrystallization
  3. temperaturewas cooled, with the crystallization
  4. additionby adding a little heptane

Quellen und Nachweise

ORD-Eintrag
ord-9dce04cd83704e3797829a7b53f6fdaa
Quelldatensatz
uspto-grants-2007_10
Patentnummer
US07285560B2

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