Reacción #3892

Ecuación de reacción

cyclohexyl isocyanate

3-[4-(4-chlorobenzyl)piperazin-1-yl]propanethiol

→

N-cyclohexyl-S-{3-[4-(4-chlorobenzyl)piperazin-1-yl]propyl}thiocarbamate dihydrochloride

Rendimiento 100.7%

Disolventes

methylene chloride

Condiciones de reacción

Tratamiento posterior

1. 1
   Concentraciónconcentrated in vacuo
2. 2
   OtroThe residue crystallized
3. 3
   OtroThe product was recrystallized from aqueous ethanol
4. 4
   workup.DISSOLUTIONdissolved in ether
5. 5
   Secadothe ethanol solution was dried (magnesium sulfate)
6. 6
   OtroThe salt was then precipitated with ethereal hydrochloric acid
7. 7
   Otrorecrystallized twice from aqueous ethanol

Procedimiento

A mixture of 1.0 g of cyclohexyl isocyanate, 2.1 g of 3-[4-(4-chlorobenzyl)piperazin-1-yl]propanethiol and 10 ml of methylene chloride was stirred at room temperature overnight and then concentrated in vacuo. The residue crystallized upon standing. The product was recrystallized from aqueous ethanol, dissolved in ether, and the ethanol solution was dried (magnesium sulfate). The salt was then precipitated with ethereal hydrochloric acid and recrystallized twice from aqueous ethanol to give 1.2 g (30% of theory) of N-cyclohexyl-S-{3-[4-(4-chlorobenzyl)piperazin-1-yl]propyl}thiocarbamate dihydrochloride as a white crystalline solid, M.p. >165° C. (dec.).

Fuente