反应 #1596940
ord-fce7cd6d5dc94a0f94cbe4a5e61c8f75
反应方程式
phenyl isothiocyanate
2-amino-2-methyl-1-propanol
→
N-(1-hydroxy-2-methylpropan-2-yl)-N′-phenylthiourea
收率 60.0%
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1workup.ADDITIONwas slowly added dropwise to the mixture over one hour
- 2workup.ADDITIONUpon completion of the addition
- 3workup.STIRRINGthe resulting mixture was stirred for 12 hours at room temperature
- 4温度The precipitated crystals were refluxed
- 5温度with heat
- 6workup.DISSOLUTIONto be dissolved
- 7其他recrystallized
- 8其他The crystals thus obtained
- 9过滤were collected by filtration
- 10洗涤washed with 20 mL of diethyl ether three times
- 11其他dried under reduced pressure at room temperature
实验过程
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%).