Реакция #1596941

Уравнение реакции

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

NaOH

→

title compound

Выход 30.2%

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

Выход 30.2%

Растворители

HCl

Условия реакции

Обработка

1. 1
   ТемператураAfter cooling
2. 2
   Экстракцияextracted with diethyl ether
3. 3
   ПромывкаThe 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
   Промывкаthe residue was washed three times with hexane
7. 7
   ДругоеThe crystals thus obtained
8. 8
   Другоеwere dried under reduced pressure at room temperature
9. 9
   Другоеrecrystallized from methanol twice

Методика

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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