반응 #3892

반응 방정식

cyclohexyl isocyanate

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

→

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

수율 100.7%

용매

methylene chloride

반응 조건

후처리

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

실험 절차

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.).

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