Methanesulfonic Acid → di[6-(N,N-diethyl)aminohexyl]3,3'-dithiodipropionate

HRID 1253400

Reaktionsgleichung

CS(O)(=O)=O.[CH2:6]([N:8]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][OH:17])[CH2:9][CH3:10])[CH3:7].[C:18]([OH:29])(=[O:28])[CH2:19][CH2:20][S:21][S:22][CH2:23][CH2:24][C:25]([OH:27])=O>C(C(C)=O)C(C)C>[CH2:9]([N:8]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][O:17][C:25](=[O:27])[CH2:24][CH2:23][S:22][S:21][CH2:20][CH2:19][C:18]([O:29][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][N:8]([CH2:9][CH3:10])[CH2:6][CH3:7])=[O:28])[CH2:6][CH3:7])[CH3:10]

Komponenten

Reaktionsbedingungen

Temperatur: 120 °C

Versuchsvorschrift

1.3 g of methanesulfonic acid (manufactured by Wako Pure Chemical Industries, Ltd.) was added dropwise, under an atmosphere of nitrogen and at 70° C., to 2.3 g of the obtained 6-(N,N-diethyl)amino-1-hexanol. After stifling for 10 minutes, 1.4 g of 3,3′-dithiodipropionic acid (manufactured by Wako Pure Chemical Industries, Ltd.) was added, and the resulting mixture was heated to 120° C. and then stirred at 110° C. for 4 hours. Following completion of the reaction, the reaction mixture was cooled to room temperature and then added gradually to 50 mL of methyl isobutyl ketone (manufactured by Wako Pure Chemical Industries, Ltd.). After stirring for 2 hours, the precipitated crystals were collected by filtration and washed with acetone, yielding the methanesulfonate salt of di[6-(N,N-diethyl)aminohexyl]3,3′-dithiodipropionate.

Aufarbeitung

customcompletion of the reaction
temperaturethe reaction mixture was cooled to room temperature
stirringAfter stirring for 2 hours
filtrationthe precipitated crystals were collected by filtration
washwashed with acetone

Quellen und Nachweise

ORD-Eintrag: ord-8d6007077784428b8f31c7e3d6b9d121
Quelldatensatz: uspto-grants-2013_06
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08455413B2

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