Реакция #94254
ord-d99c0a11a40042bca44c584cad17064a
Уравнение реакции
cyclohexyl isocyanate
1,3-dimethyl-3-hydroperoxybutyl alcohol
→
colorless solid
Выход 39.0%
1,3-Dimethyl-3-(N-cyclohexyl-carbamoylperoxy)butyl N-cyclohexylcarbamate
Выход 39.0%
Растворители
Условия реакции
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1workup.ADDITIONA mixture of 18.7 g
- 2ДругоеThe reaction vessel was protected with a calcium chloride tube
- 3Фильтрацияfiltered
- 4ПромывкаThe filter cake was washed with an additional 30 ml of ether and air
- 5Другоеdried
Методика
A mixture of 18.7 g. (0.15 mole) of cyclohexyl isocyanate, 6.7 g. (0.05 mole) of 1,3-dimethyl-3-hydroperoxybutyl alcohol and 3 drops of triethylamine was stirred for 5 days at ambient temperature. The reaction vessel was protected with a calcium chloride tube to keep out moisture. Within 2 days, a solid began to appear, and after the 5 day stirring period the reaction mixture was stripped in vacuo. The residue was slurried in 100 ml of ether and filtered. The filter cake was washed with an additional 30 ml of ether and air dried. A total of 7.5 grams of a colorless solid was obtained.