Reaktion #417580

Reaktionsgleichung

[(2-chloroethyl)sulfonyl]benzene

4-(N,N-diethylamino)-1-butanamine

oxalic acid

→

title compound

Ausbeute 164.4%

N,N-Diethyl-N'-[2-(phenylsulfonyl)ethyl]-1,4-butanediamine oxalate hydrate

Ausbeute 164.4%

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe solvent was removed in vacuo
2. 2
   Sonstigethe residue was partitioned between methylene chloride and dilute sodium hydroxide
3. 3
   TrocknenThe methylene chloride solution was dried over magnesium sulfate
4. 4
   Sonstigethe solvent was removed in vacuo
5. 5
   workup.DISSOLUTIONThe residue was dissolved in methanol
6. 6
   Sonstigea precipitate was collected

Vorschrift

A mixture of 28.2 g (0.138 mole) of [(2-chloroethyl)sulfonyl]benzene and 20.0 g (0.139 mole) of 4-(N,N-diethylamino)-1-butanamine in 700 ml of acetonitrile was stirred at room temperature for 16 hr. The solvent was removed in vacuo, and the residue was partitioned between methylene chloride and dilute sodium hydroxide. The methylene chloride solution was dried over magnesium sulfate, and the solvent was removed in vacuo. The residue was dissolved in methanol, a solution of 25.0 g (0.278 mole) of oxalic acid was added and a precipitate was collected to give 47.69 g (68.9%) of title compound, a white crystalline solid, mp 158°-165° C. with decomposition.

Quelle