Reacción #1340583

Ecuación de reacción

4,4′-dithiodibutyric acid

methanesulfonic acid

6-amino-1-hexanol

→

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

Disolventes

methyl isobutyl ketone

Condiciones de reacción

Tratamiento posterior

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

Procedimiento

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.

Fuente