反応 #1596941

反応方程式

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

NaOH

→

title compound

収率 30.2%

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

収率 30.2%

溶媒

HCl

反応条件

後処理

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

実験手順

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%).

出典