Reaktion #1596940

Reaktionsgleichung

phenyl isothiocyanate

2-amino-2-methyl-1-propanol

→

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

Ausbeute 60.0%

Lösungsmittel

chloroform

chloroform

Reaktionsbedingungen

Aufarbeitung

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
   TemperaturThe precipitated crystals were refluxed
5. 5
   Temperaturwith heat
6. 6
   workup.DISSOLUTIONto be dissolved
7. 7
   Sonstigerecrystallized
8. 8
   SonstigeThe crystals thus obtained
9. 9
   Filtrationwere collected by filtration
10. 10
    Waschenwashed with 20 mL of diethyl ether three times
11. 11
    Sonstigedried under reduced pressure at room temperature

Vorschrift

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%).

Quelle