Triethylamine → HCID 57916246, Verbindung

HRID 2059891Notizen

Reaktionsgleichung

[Cl:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([S:9](Cl)(=[O:11])=[O:10])=[C:4]([CH3:13])[CH:3]=1.Cl.[CH2:15]([O:17][C:18](=[O:29])[CH:19](CC)[CH2:20][CH:21]1[CH2:26][CH2:25][CH2:24][CH2:23][NH:22]1)[CH3:16].C(N(CC)CC)C>ClCCl>[CH2:15]([O:17][C:18](=[O:29])[CH2:19][CH2:20][CH:21]1[CH2:26][CH2:25][CH2:24][CH2:23][N:22]1[S:9]([C:5]1[CH:6]=[C:7]([CH3:8])[C:2]([Cl:1])=[CH:3][C:4]=1[CH3:13])(=[O:11])=[O:10])[CH3:16]

Komponenten

Reaktionsbedingungen

Temperatur: 0 °C

Versuchsvorschrift

4-Chloro-2,5-dimethyl-benzenesulfonyl chloride (1 g, 3.8 mmol) was added to a solution of ethyl 3-(piperidin-2-yl)propionic acid ethyl ester hydrochloride (1.1 g, 4.6 mmol) in dichloromethane (15 ml) while stirring, the mixture was cooled to 0° C., and triethylamine (1.6 ml, 11.5 mmol) was added dropwise over 15 min. The mixture was stirred for 4 h at 0° C., then diluted with dichloromethane, washed with water and saturated sodium chloride solution, dried over sodium sulfate and concentrated to small volume under vacuum. The crude product was purified with ethyl acetate/hexane (9:1) by column chromatography. Yield: 50%

Aufarbeitung

stirringThe mixture was stirred for 4 h at 0° C.
washwashed with water and saturated sodium chloride solution
dry with materialdried over sodium sulfate
concentrationconcentrated to small volume under vacuum
customThe crude product was purified with ethyl acetate/hexane (9:1) by column chromatography

Quellen und Nachweise

ORD-Eintrag: ord-ead2b3f713d34cbfbc1e1ea7f42b6c55
Quelldatensatz: uspto-grants-2012_10
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08278319B2

Notizen zur Reaktion

Wird geladen…