Triethylamine → 3-Ethyl-2-ethylimino-4-(4-chloro-3-sulfamoylphenyl)-1,3-thiazolidine-4-ol-hydrochloride

HRID 461111

Reaktionsgleichung

Br.[CH2:2]([N:4]1[C:8]([C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]([S:17](=[O:20])(=[O:19])[NH2:18])[CH:11]=2)([OH:9])[CH2:7][S:6][C:5]1=[N:21][CH2:22][CH3:23])[CH3:3].C(N(CC)CC)C>CO>[ClH:16].[CH2:2]([N:4]1[C:8]([C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]([S:17](=[O:20])(=[O:19])[NH2:18])[CH:11]=2)([OH:9])[CH2:7][S:6][C:5]1=[N:21][CH2:22][CH3:23])[CH3:3]

Komponenten

Reaktionsbedingungen

Temperatur: 40 °C

Versuchsvorschrift

17 g of 3-ethyl-2-ethylimino-4-(4-chloro-3-sulfamoylphenyl)-1,3-thiazolidine-4-ol-hydrobromide were suspended in 100 ml of methanol and shortly heated to boiling after the addition of 10 ml of triethyl amine. The solvent was distilled off under reduced pressure, 150 ml of water were added to the residue and the mixture was extracted with 200 ml of ethyl acetate. After drying the organic phase over sodium sulfate the solvent was distilled off under reduced pressure. The residue was dissolved in 100 ml of acetone, the solution was acidified with 15% ethanolic HCl and the oily precipitate of the end product was crystallized with acetone heated to 40° C.

Aufarbeitung

temperatureshortly heated
distillationThe solvent was distilled off under reduced pressure, 150 ml of water
additionwere added to the residue
extractionthe mixture was extracted with 200 ml of ethyl acetate
dry with materialAfter drying the organic phase over sodium sulfate the solvent
distillationwas distilled off under reduced pressure
dissolutionThe residue was dissolved in 100 ml of acetone
customthe oily precipitate of the end product was crystallized with acetone

Quellen und Nachweise

ORD-Eintrag: ord-4fbf59d8134e4cd6a7123834d08ab33b
Quelldatensatz: uspto-grants-1977_12
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US04061761

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