Reaktionsgleichung
[CH:1]1([N:7]=[C:8]=[O:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Cl:10][C:11]1[CH:27]=[CH:26][C:14]([CH2:15][N:16]2[CH2:21][CH2:20][N:19]([CH2:22][CH2:23][CH2:24][SH:25])[CH2:18][CH2:17]2)=[CH:13][CH:12]=1>C(Cl)Cl>[ClH:10].[ClH:10].[CH:1]1([NH:7][C:8](=[SH:25][CH2:24][CH2:23][CH2:22][N:19]2[CH2:20][CH2:21][N:16]([CH2:15][C:14]3[CH:13]=[CH:12][C:11]([Cl:10])=[CH:27][CH:26]=3)[CH2:17][CH2:18]2)[OH:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
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.).
Aufarbeitung
- concentrationconcentrated in vacuo
- customThe residue crystallized
- customThe product was recrystallized from aqueous ethanol
- dissolutiondissolved in ether
- dry with materialthe ethanol solution was dried (magnesium sulfate)
- customThe salt was then precipitated with ethereal hydrochloric acid
- customrecrystallized twice from aqueous ethanol
Quellen und Nachweise
- ORD-Eintrag
- ord-9d1937c896e54cb4b8977e4368ead391
- Quelldatensatz
- uspto-grants-1988_02
- Patentnummer
- US04722926
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