Reaktion #1596941

Reaktionsgleichung

N-(1-hydroxy-2-methylpropan-2-yl)-N′-phenylthiourea

NaOH

→

title compound

Ausbeute 30.2%

4,4-dimethyl-N-phenyl-4,5-dihydrothiazol-2-amine

Ausbeute 30.2%

Lösungsmittel

HCl

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturAfter cooling
2. 2
   Extraktionextracted with diethyl ether
3. 3
   WaschenThe extract was washed with saturated brine
4. 4
   workup.ADDITIONanhydrous sodium sulfate was added
5. 5
   workup.DISTILLATIONThe organic phase was distilled off under reduced pressure
6. 6
   Waschenthe residue was washed three times with hexane
7. 7
   SonstigeThe crystals thus obtained
8. 8
   Sonstigewere dried under reduced pressure at room temperature
9. 9
   Sonstigerecrystallized from methanol twice

Vorschrift

N-(1-hydroxy-2-methylpropan-2-yl)-N′-phenylthiourea (80.1 g, 0.36 mol) was dissolved in 2,400 mL of 35% HCl, and the resulting mixture was stirred while heating at 90° C. for 1.5 hours. After cooling, the mixture was neutralized with NaOH and extracted with diethyl ether. The extract was washed with saturated brine and then anhydrous sodium sulfate was added. The organic phase was distilled off under reduced pressure and the residue was washed three times with hexane. The crystals thus obtained were dried under reduced pressure at room temperature, and then recrystallized from methanol twice to give 22.4 g of the title compound (yield 18%).

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