Реакция #3892

Уравнение реакции

cyclohexyl isocyanate

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

→

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

Выход 100.7%

Растворители

methylene chloride

Условия реакции

Обработка

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

Методика

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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