反応 #3892

反応方程式

cyclohexyl isocyanate

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

→

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

収率 100.7%

溶媒

methylene chloride

反応条件

後処理

1. 1
   濃縮concentrated in vacuo
2. 2
   その他The residue crystallized
3. 3
   その他The product was recrystallized from aqueous ethanol
4. 4
   workup.DISSOLUTIONdissolved in ether
5. 5
   乾燥the ethanol solution was dried (magnesium sulfate)
6. 6
   その他The salt was then precipitated with ethereal hydrochloric acid
7. 7
   その他recrystallized twice from aqueous ethanol

実験手順

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.).

出典