Reaktionsgleichung
[C:1]1([S:7]([CH2:10][CH2:11][Cl:12])(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:13]([O:15][CH2:16][CH2:17][CH2:18][NH2:19])[CH3:14].C(N(CC)CC)C.Cl>C(#N)C.CO.CCOCC>[ClH:12].[CH2:13]([O:15][CH2:16][CH2:17][CH2:18][NH:19][CH2:11][CH2:10][S:7]([C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)(=[O:9])=[O:8])[CH3:14]Komponenten
8
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 3
Versuchsvorschrift
A mixture of 51.4 g (0.253 mole) of 2-chloroethyl phenyl sulfone, 50.2 g (0.417 mole) of 3-ethoxy-1-propanamine, and 33.0 g (0.327 mole) of triethylamine in 400 ml of acetonitrile was stirred at room temperature for 20 hr. The solvent was removed in vacuo and the residue was partitioned between methylene chloride and dilute sodium hydroxide. The methylene chloride phase was dried over magnesium sulfate, and the solvent was removed in vacuo to give an oil. This was dissolved in methanol, an excess of ethereal hydrogen chloride was added and ether was added. A precipitate was collected to give 49.2 g (63.2%) of white crystalline solid, m.p. 169°-170° C.
Aufarbeitung
- customThe solvent was removed in vacuo
- customthe residue was partitioned between methylene chloride and dilute sodium hydroxide
- dry with materialThe methylene chloride phase was dried over magnesium sulfate
- customthe solvent was removed in vacuo
- customto give an oil
- customA precipitate was collected
Quellen und Nachweise
- ORD-Eintrag
- ord-b9ffe40dfc354894b3753bf7aa940b3d
- Quelldatensatz
- uspto-grants-1988_02
- Patentnummer
- US04724235
Verknüpfte Notizen
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