Acrylonitrile → HCID 70631280, Verbindung

HRID 259116Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 259116
[C:1](#[N:4])[CH:2]=[CH2:3].[CH3:5][O:6][CH:7]1[C:16]2[CH2:15][CH2:14][CH2:13][CH:12]3[CH2:17][CH2:18][O:19][C:10]([C:11]=23)=[CH:9][N:8]1[O:20][CH3:21].[OH-].[Na+]>O1CCOCC1>[C:1]([CH2:2][CH2:3][CH:14]1[CH2:15][C:16]2[CH:7]([O:6][CH3:5])[N:8]([O:20][CH3:21])[CH:9]=[C:10]3[O:19][CH2:18][CH2:17][CH:12]([C:11]=23)[CH2:13]1)#[N:4]

Komponenten

5

Edukt 3

HCID 7855AcrylonitrileHCID 14798Sodium HydroxideHCID 20523931HCID 20523931, Verbindung

Produkt 1

HCID 70631280HCID 70631280, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A solution of acrylonitrile (12 ml) and 1,2,3a,4,5,6-hexahydro-7,8-dimethoxypyrano[2,3,4-de]isoquinoline (11 g), described in Example 56, in dioxane (80 ml) and 10% NaOH solution (2.5 ml) is heated and stirred on the steam bath for 24 hr. The mixture is evaporated and the residue is dissolved in a mixture of ether and a little chloroform. The solution is extracted with 2N HCl and the extracts are washed (brine), dried and evaporated. The residue is crystallized from ether and then from benzene-hexane to give the title compound, m.p. 105°-107° C.

Aufarbeitung

  1. customThe mixture is evaporated
  2. dissolutionthe residue is dissolved in a mixture of ether
  3. extractionThe solution is extracted with 2N HCl
  4. washthe extracts are washed (brine)
  5. customdried
  6. customevaporated
  7. customThe residue is crystallized from ether

Quellen und Nachweise

ORD-Eintrag
ord-93bb737e32da4709a20e36224059ef9a
Quelldatensatz
uspto-grants-1977_07
Patentnummer
US04036842

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