Reaktion #4304

Reaktionsgleichung

N-[2-(phenylthio)ethyl]-2-propanamine hydrochloride

sodium perborate tetrahydrate

sodium hydroxide

→

white solid

Ausbeute 177.6%

N-[-(Phenylsulfinyl)ethyl]-2-propanamine maleate

Ausbeute 177.6%

Lösungsmittel

sulfuric acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionthe basic solution was extracted with methylene chloride
2. 2
   TrocknenThe methylene chloride solution was dried over magnesium sulfate
3. 3
   Sonstigethe solvent was removed in vacuo
4. 4
   workup.DISSOLUTIONThe residue was dissolved in ether
5. 5
   workup.ADDITIONa solution of maleic acid in methanol was added
6. 6
   Sonstigeprecipitated

Vorschrift

A solution of 15.62 g (0.067 mole) of N-[2-(phenylthio)ethyl]-2-propanamine hydrochloride and 15.62 g (0.101 mole) of sodium perborate tetrahydrate in 300 ml of 2M sulfuric acid was stirred at room temperature for 16 hr. The solution was made basic with 50% sodium hydroxide, and the basic solution was extracted with methylene chloride. The methylene chloride solution was dried over magnesium sulfate, and the solvent was removed in vacuo. The residue was dissolved in ether, a solution of maleic acid in methanol was added, and precipitated to give 19.48 g (88.3%) of white solid, m.p. 102.5°-103.5° C. A sample of this was recrystallized from methanol-ether, m.p. 102.5°-103.5° C.

Quelle