تفاعل #1596941

معادلة التفاعل

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

NaOH

→

title compound

المردود 30.2%

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

المردود 30.2%

المذيبات

HCl

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter cooling
2. 2
   استخلاصextracted with diethyl ether
3. 3
   غسيلThe 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
   غسيلthe residue was washed three times with hexane
7. 7
   أخرىThe crystals thus obtained
8. 8
   أخرىwere dried under reduced pressure at room temperature
9. 9
   أخرىrecrystallized from methanol twice

الإجراء التجريبي

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%).

المصدر