تفاعل #1596940
ord-fce7cd6d5dc94a0f94cbe4a5e61c8f75
معادلة التفاعل
phenyl isothiocyanate
2-amino-2-methyl-1-propanol
→
N-(1-hydroxy-2-methylpropan-2-yl)-N′-phenylthiourea
المردود 60.0%
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 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
- 4درجة الحرارةThe precipitated crystals were refluxed
- 5درجة الحرارةwith heat
- 6workup.DISSOLUTIONto be dissolved
- 7أخرىrecrystallized
- 8أخرىThe crystals thus obtained
- 9ترشيحwere collected by filtration
- 10غسيلwashed with 20 mL of diethyl ether three times
- 11أخرىdried under reduced pressure at room temperature
الإجراء التجريبي
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%).