Reacción #658779

ord-0668a5a0741b4e9b93abf1899e8ce733

Ecuación de reacción

CC(N)CNCC(C)N
di-(2-aminopropyl)amine
S=C=S
Carbon disulfide
S
hydrogen sulfide
CC1CN2CC(C)NC2=N1
2,6-Dimethyl-2,3,5,6-tetrahydro-1H-imidazo[1,2-a]imidazole

Condiciones de reacción

Temperatura
200°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroThe solvent was then removed by distillation
  2. 2
    workup.DISSOLUTIONThe product was then dissolved in approximately 5 mL of hexanes
  3. 3
    workup.ADDITION0.5 mL of a 2.0 M ether solution of hydrogen chloride was added

Procedimiento

In a 100 mL flask, 0.4078 g of di-(2-aminopropyl)amine (0.00311 mol) was dissolved in 50 mL of 1-methylnaphthalene. Carbon disulfide (0.18 mL, 0.00298 mol) was added. The reaction was stirred for three hours then heated to 200° C. The reaction was heated for four days until production of hydrogen sulfide stopped. The solvent was then removed by distillation. The product was then dissolved in approximately 5 mL of hexanes and 0.5 mL of a 2.0 M ether solution of hydrogen chloride was added. The yield of the precipitate was 0.278 g (53%). The NMR had a doublet at 1.19 ppm, a multiplet at 3.44 ppm, a multiplet at 3.92 ppm and a multiplet at 4.15 ppm.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US09029189B2uspto-grants-2015_05