Реакция #94254

ord-d99c0a11a40042bca44c584cad17064a

Уравнение реакции

O=C=NC1CCCCC1
cyclohexyl isocyanate
CC(O)CC(C)(C)OO
1,3-dimethyl-3-hydroperoxybutyl alcohol
CC(CC(C)(C)OOC(=O)NC1CCCCC1)OC(=O)NC1CCCCC1
colorless solid
Выход 39.0%
CC(CC(C)(C)OOC(=O)NC1CCCCC1)OC(=O)NC1CCCCC1
1,3-Dimethyl-3-(N-cyclohexyl-carbamoylperoxy)butyl N-cyclohexylcarbamate
Выход 39.0%

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONA mixture of 18.7 g
  2. 2
    ДругоеThe reaction vessel was protected with a calcium chloride tube
  3. 3
    Фильтрацияfiltered
  4. 4
    ПромывкаThe filter cake was washed with an additional 30 ml of ether and air
  5. 5
    Другоеdried

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04129700uspto-grants-1978_12