تفاعل #3892

معادلة التفاعل

cyclohexyl isocyanate

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

→

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

المردود 100.7%

المذيبات

methylene chloride

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.).

المصدر