Реакция #1596940

ord-fce7cd6d5dc94a0f94cbe4a5e61c8f75

Уравнение реакции

S=C=Nc1ccccc1
phenyl isothiocyanate
CC(C)(N)CO
2-amino-2-methyl-1-propanol
CC(C)(CO)NC(=S)Nc1ccccc1
N-(1-hydroxy-2-methylpropan-2-yl)-N′-phenylthiourea
Выход 60.0%

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  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
    ТемператураThe precipitated crystals were refluxed
  5. 5
    Температураwith heat
  6. 6
    workup.DISSOLUTIONto be dissolved
  7. 7
    Другоеrecrystallized
  8. 8
    ДругоеThe crystals thus obtained
  9. 9
    Фильтрацияwere collected by filtration
  10. 10
    Промывкаwashed with 20 mL of diethyl ether three times
  11. 11
    Другоеdried under reduced pressure at room temperature

Методика

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%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08211412B2uspto-grants-2012_07