Iodoethane → HCID 9799580, Verbindung

HRID 567063Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 567063
[CH2:1]([N:3]([CH:8]1[C:17]2[C:12](=[CH:13][CH:14]=[C:15]([O:18][CH2:19][CH2:20][OH:21])[CH:16]=2)[O:11][C:10]([CH3:23])([CH3:22])[CH2:9]1)[S:4]([CH3:7])(=[O:6])=[O:5])[CH3:2].[H-].[Na+].[CH2:26](I)[CH3:27]>CC(N(C)C)=O>[CH2:26]([O:21][CH2:20][CH2:19][O:18][C:15]1[CH:16]=[C:17]2[C:12](=[CH:13][CH:14]=1)[O:11][C:10]([CH3:22])([CH3:23])[CH2:9][CH:8]2[N:3]([CH2:1][CH3:2])[S:4]([CH3:7])(=[O:5])=[O:6])[CH3:27]

Komponenten

5

Edukt 3

HCID 6340IodoethaneHCID 24758Sodium hydrideHCID 9841033HCID 9841033, Verbindung

Produkt 1

HCID 9799580HCID 9799580, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 31374DimethylacetamideLösungsmittel

Versuchsvorschrift

2.3 g (6.7 mmol) of N-ethyl-N-[6-(2-hydroxyethoxy)-2,2-dimethylchroman-4-yl]methanesulfonamide (Example 8) were alkylated with 0.48 g (about 10 mmol) of NaH (80 percent dispersion) and 1.6 ml (about 20 mmol) of ethyl iodide in 50 ml of DMA under nitrogen. After working up and purification by column chromatography on silica gel, 1.0 g of the title compound was crystallized from corresponding fractions using petroleum ether, m.p. 73-75° C.

Aufarbeitung

  1. custompurification by column chromatography on silica gel, 1.0 g of the title compound
  2. customwas crystallized from corresponding fractions

Quellen und Nachweise

ORD-Eintrag
ord-70874595e67543849b090c00902e1f06
Quelldatensatz
uspto-grants-2001_01
Patentnummer
US06177449B1

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