反应 #1596941

反应方程式

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

NaOH

→

title compound

收率 30.2%

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

收率 30.2%

溶剂

HCl

反应条件

后处理

1. 1
   温度After cooling
2. 2
   萃取extracted with diethyl ether
3. 3
   洗涤The 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
   洗涤the residue was washed three times with hexane
7. 7
   其他The crystals thus obtained
8. 8
   其他were dried under reduced pressure at room temperature
9. 9
   其他recrystallized from methanol twice

实验过程

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%).

来源