Reaktion #1340583

Reaktionsgleichung

4,4′-dithiodibutyric acid

methanesulfonic acid

6-amino-1-hexanol

→

di(6-aminohexyl) 4,4′-dithiodibutyrate

Lösungsmittel

methyl isobutyl ketone

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGstirred at 110° C. for 4 hours
2. 2
   Sonstigecompletion of the reaction
3. 3
   Temperaturthe reaction mixture was cooled to room temperature
4. 4
   workup.STIRRINGAfter stirring for 2 hours
5. 5
   Filtrationthe precipitated crystals were collected by filtration
6. 6
   Waschenwashed with acetone

Vorschrift

5.1 g of methanesulfonic acid (manufactured by Wako Pure Chemical Industries, Ltd.) was added dropwise, under an atmosphere of nitrogen and at 70° C., to 5.9 g of 6-amino-1-hexanol. After stirring for 10 minutes, 6.0 g of 4,4′-dithiodibutyric acid (manufactured by Tokyo Chemical Industry Co., 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-aminohexyl) 4,4′-dithiodibutyrate.

Quelle