반응 #1596941

반응 방정식

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

NaOH

→

title compound

수율 30.2%

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

수율 30.2%

용매

HCl

반응 조건

후처리

1. 1
   온도After cooling
2. 2
   추출extracted with diethyl ether
3. 3
   세척The 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
   세척the residue was washed three times with hexane
7. 7
   기타The crystals thus obtained
8. 8
   기타were dried under reduced pressure at room temperature
9. 9
   기타recrystallized from methanol twice

실험 절차

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%).

출처