반응 #1596940

반응 방정식

phenyl isothiocyanate

2-amino-2-methyl-1-propanol

→

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

수율 60.0%

용매

chloroform

chloroform

반응 조건

후처리

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
   온도The precipitated crystals were refluxed
5. 5
   온도with heat
6. 6
   workup.DISSOLUTIONto be dissolved
7. 7
   기타recrystallized
8. 8
   기타The crystals thus obtained
9. 9
   여과were collected by filtration
10. 10
    세척washed with 20 mL of diethyl ether three times
11. 11
    기타dried under reduced pressure at room temperature

실험 절차

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%).

출처