反応 #1596940

反応方程式

phenyl isothiocyanate

2-amino-2-methyl-1-propanol

→

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

収率 60.0%

溶媒

chloroform

chloroform

反応条件

後処理

1. 1
   workup.ADDITIONwas slowly added dropwise to the mixture over one hour
2. 2
   workup.ADDITIONUpon completion of the addition
3. 3
   workup.STIRRINGthe resulting mixture was stirred for 12 hours at room temperature
4. 4
   温度The precipitated crystals were refluxed
5. 5
   温度with heat
6. 6
   workup.DISSOLUTIONto be dissolved
7. 7
   その他recrystallized
8. 8
   その他The crystals thus obtained
9. 9
   ろ過were collected by filtration
10. 10
    洗浄washed with 20 mL of diethyl ether three times
11. 11
    その他dried under reduced pressure at room temperature

実験手順

In 500 g of chloroform was dissolved 2-amino-2-methyl-1-propanol (61.6 g, 0.69 moL). Then, 300 g of chloroform solution containing phenyl isothiocyanate (81.6 g, 0.6 moL) was slowly added dropwise to the mixture over one hour, while stirring. Upon completion of the addition, the resulting mixture was stirred for 12 hours at room temperature. The precipitated crystals were refluxed with heat to be dissolved and then recrystallized. The crystals thus obtained were collected by filtration, washed with 20 mL of diethyl ether three times, and then dried under reduced pressure at room temperature to give 80.1 g of N-(1-hydroxy-2-methylpropan-2-yl)-N′-phenylthiourea (yield 60%).

出典