Dimethylamine, hydrochloride → HCID 18348536, Verbindung

HRID 2268474

Reaktionsgleichung

Reaktionsgleichung von HRID 2268474
I[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH:10]1[CH2:18][C:17]2[C:12](=[C:13]([O:25][CH3:26])[C:14]([O:23][CH3:24])=[C:15]([O:21][CH3:22])[C:16]=2[O:19][CH3:20])[CH2:11]1.Cl.[CH3:28][NH:29][CH3:30].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C.O>[CH3:26][O:25][C:13]1[C:14]([O:23][CH3:24])=[C:15]([O:21][CH3:22])[C:16]([O:19][CH3:20])=[C:17]2[C:12]=1[CH2:11][CH:10]([CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][N:29]([CH3:30])[CH3:28])[CH2:18]2

Komponenten

6

Edukt 3

HCID 10473Dimethylamine, hydrochlorideHCID 11430Potassium CarbonateHCID 183485412-(8-Iodooctyl)-4,5,6,7-tetramethoxyindan

Produkt 1

HCID 18348536HCID 18348536, VerbindungAusbeute 62,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

The mixture of 2-(8-iodooctyl)-4,5,6,7-tetramethoxyindan (1.20 g), dimethylamine hydrochloride (411 mg) and potassium carbonate (1.74 g) in DMF (12 ml) was stirred at room temperature for 12 hr. The reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride and dried. The solvent was removed in vacuo. The residue was purified by alumina column chromatography (hexane to hexane:ethyl acetate=10:1) to yield the entitled compound (620 mg) as an oil.

Aufarbeitung

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with water and saturated aqueous sodium chloride
  3. customdried
  4. customThe solvent was removed in vacuo
  5. customThe residue was purified by alumina column chromatography (hexane to hexane:ethyl acetate=10:1)

Quellen und Nachweise

ORD-Eintrag
ord-f3f77029c0d34110af48b9634745dd60
Quelldatensatz
uspto-grants-2001_12
Patentnummer
US06326369B1

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