Potassium Iodide → HCID 70290042, Verbindung

HRID 369767

Reaktionsgleichung

Reaktionsgleichung von HRID 369767
[NH2:1][CH2:2][CH2:3][N:4]1[CH2:9][CH2:8][N:7]([C:10]2[C:19]3[O:18][CH2:17][CH2:16][O:15][C:14]=3[CH:13]=[CH:12][CH:11]=2)[CH2:6][CH2:5]1.BrC[CH:22]=[O:23].[I-].[K+].C(=O)([O-])[O-].[K+].[K+].O1[CH2:37][CH2:36][O:35][CH2:34]C1>C(OCC)(=O)C.CO.O>[O:15]1[C:14]2[CH:13]=[CH:12][CH:11]=[C:10]([N:7]3[CH2:6][CH2:5][N:4]([CH2:3][CH2:2][NH:1][CH2:37][CH:36]([O:35][CH3:34])[O:23][CH3:22])[CH2:9][CH2:8]3)[C:19]=2[O:18][CH2:17][CH2:16]1

Komponenten

8

Edukt 5

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 312751,4-DioxaneHCID 105131Acetaldehyde, bromo-HCID 10587641HCID 10587641, Verbindung

Produkt 1

HCID 70290042HCID 70290042, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 21584119Ethylacetate methanolLösungsmittel

Versuchsvorschrift

A mixture of 1-(2-amino-1-ethyl)-4-(1,4-benzodioxan-5-yl)piperazine (9.1 g), bromoacetaldehyde dimethylacetale (6.5 g), potassium iodide (0.5 g), and potassium carbonate (4.8 g) in 1,4-dioxan (200 ml) was refluxed for 16 h. Water was added followed by extraction with ethyl acetate. The organic phase was concentrated in vacuo leaving an oil which was applied to a silica gel column (eluent: ethyl acetate/methanol=1:3). The product, 1-(1,4-benzodioxan-5-yl)-4-[2-(2,2-dimethoxy-1-ethylamino)-1-ethyl]piperazine, was obtained as an oil (4.7 g).

Aufarbeitung

  1. temperaturewas refluxed for 16 h
  2. extractionfollowed by extraction with ethyl acetate
  3. concentrationThe organic phase was concentrated in vacuo
  4. customleaving an oil which

Quellen und Nachweise

ORD-Eintrag
ord-a9408372408f465faf1f6e2346ffb2fa
Quelldatensatz
uspto-grants-2000_10
Patentnummer
US06140331

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