Thiophosgene → 4-Ethoxycarbonyl-1-piperazinylthiocarbonyl chloride

HRID 1462445Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1462445
[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° is 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 is allowed to warm up to room temperature overnight. The suspension is filtered and the filtrate is evaporated to dryness. The residue is crystallized from methylene chloridehexane to give 4-ethoxycarbonyl-1-piperazinylthiocarbonyl chloride, m.p. 107°-111°.

Aufarbeitung

  1. additionis added
  2. filtrationThe suspension is filtered
  3. customthe filtrate is evaporated to dryness
  4. customThe residue is crystallized from methylene chloridehexane

Quellen und Nachweise

ORD-Eintrag
ord-cb570bf3d6be410db649bcca16b3a93c
Quelldatensatz
uspto-grants-1984_07
Patentnummer
US04460587

Notizen zur Reaktion

Wird geladen…