Reacción #94254

ord-d99c0a11a40042bca44c584cad17064a

Ecuación de reacción

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
Rendimiento 39.0%
CC(CC(C)(C)OOC(=O)NC1CCCCC1)OC(=O)NC1CCCCC1
1,3-Dimethyl-3-(N-cyclohexyl-carbamoylperoxy)butyl N-cyclohexylcarbamate
Rendimiento 39.0%

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONA mixture of 18.7 g
  2. 2
    OtroThe reaction vessel was protected with a calcium chloride tube
  3. 3
    Filtraciónfiltered
  4. 4
    LavadoThe filter cake was washed with an additional 30 ml of ether and air
  5. 5
    Otrodried

Procedimiento

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.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04129700uspto-grants-1978_12