반응 #4304

반응 방정식

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

sodium perborate tetrahydrate

sodium hydroxide

→

white solid

수율 177.6%

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

수율 177.6%

용매

sulfuric acid

반응 조건

후처리

1. 1
   추출the basic solution was extracted with methylene chloride
2. 2
   건조The methylene chloride solution was dried over magnesium sulfate
3. 3
   기타the 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
   기타precipitated

실험 절차

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.

출처