Reacción #1340584

Ecuación de reacción

3,3′-dithiodipropionic acid

methanesulfonic acid

2-amino-1-hexanol

→

di(2-aminohexyl) 3,3′-dithiodipropionate

Disolventes

methyl isobutyl ketone

Condiciones de reacción

Tratamiento posterior

1. 1
   Otrocompletion of the reaction
2. 2
   Temperaturathe reaction mixture was cooled to room temperature
3. 3
   workup.WAITAfter stifling for 1 hour
4. 4
   Filtraciónthe precipitated crystals were collected by filtration
5. 5
   Otrodried at 50° C.

Procedimiento

6.1 g of methanesulfonic acid (manufactured by Wako Pure Chemical Industries, Ltd.) was added dropwise, under an atmosphere of nitrogen and at 70° C., to 7.0 g of 2-amino-1-hexanol (manufactured by Aldrich Co., Ltd.). After stifling for 10 minutes, 6.3 g of 3,3′-dithiodipropionic acid (manufactured by Wako Pure Chemical Industries, Ltd.) was added, and the resulting mixture was heated to 120° C. The mixture was then stirred at 120 to 129° C. for a further 3 hours. Following completion of the reaction, the reaction mixture was cooled to room temperature and then added gradually to 100 mL of methyl isobutyl ketone (manufactured by Wako Pure Chemical Industries, Ltd.). After stifling for 1 hour, the precipitated crystals were collected by filtration and dried at 50° C., yielding the methanesulfonate salt of di(2-aminohexyl) 3,3′-dithiodipropionate.

Fuente