Thiophosgene → 4-Ethoxycarbonyl-1-piperazinylthiocarbonyl chloride

HRID 1462334Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1462334
[C:1]([Cl:4])(Cl)=[S:2].[CH2:5]([O:7][C:8]([N:10]1[CH2:15][CH2:14][N:13]([Si](C)(C)C)[CH2:12][CH2:11]1)=[O:9])[CH3:6]>C(OCC)C>[CH2:5]([O:7][C:8]([N:10]1[CH2:11][CH2:12][N:13]([C:1]([Cl:4])=[S:2])[CH2:14][CH2:15]1)=[O:9])[CH3:6]

Komponenten

4

Edukt 2

HCID 10040ThiophosgeneHCID 133449251-Ethoxycarbonyl-4-trimethylsilylpiperazine

Produkt 1

HCID 133449264-Ethoxycarbonyl-1-piperazinylthiocarbonyl chloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel2×

Versuchsvorschrift

To a solution of 4.66 ml of 85% thiophosgene in 200 ml of ethyl ether, cooled to -76° was added, while stirring and under nitrogen, a solution of 7 g of 1-ethoxycarbonyl-4-trimethylsilylpiperazine in 35 ml of ethyl ether over a period of 20 minutes. The mixture was allowed to warm up to room temperature overnight. The suspension was filtered and the filtrate was evaporated to dryness. The residue was crystallized from methylene chloride-hexane to give 4-ethoxycarbonyl-1-piperazinylthiocarbonyl chloride, m.p. 107°-111°.

Aufarbeitung

  1. additionwas added
  2. filtrationThe suspension was filtered
  3. customthe filtrate was evaporated to dryness
  4. customThe residue was crystallized from methylene chloride-hexane

Quellen und Nachweise

ORD-Eintrag
ord-74158b3790fc4545a26d3fce5ab905f5
Quelldatensatz
uspto-grants-1984_07
Patentnummer
US04460508

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