Reaktion #2257261

Reaktionsgleichung

Succinic acid

3-(3-{2-[(E)-3,5-diamino-6-chloro-pyrazine-2-carbonylimino]-1,3,8-triaza-spiro[4.5]decane-8-carbonyl}-benzenesulfonylamino)-propionic acid dipropylcarbamoylmethyl ester

→

title compound

3-(3-{2-[(E)-3,5-Diamino-6-chloro-pyrazine-2-carbonylimino]-1,3,8-triaza-spiro[4.5]decane-8-carbonyl}-benzenesulfonylamino)-propionic acid dipropylcarbamoylmethyl ester succinate salt

Lösungsmittel

acetonitrile

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeCrystallisation
2. 2
   Sonstigeto occur at an internal temperature of ˜30° C
3. 3
   FiltrationThe crystals were collected by filtration
4. 4
   Waschenthe filter cake washed with acetonitrile/water (95:5)
5. 5
   Sonstigedried at 50° C. under vacuum

Vorschrift

Succinic acid (409 mg, 3.47 mmol) was added to a solution of 3-(3-{2-[(E)-3,5-diamino-6-chloro-pyrazine-2-carbonylimino]-1,3,8-triaza-spiro[4.5]decane-8-carbonyl}-benzenesulfonylamino)-propionic acid dipropylcarbamoylmethyl ester (step 1, Method B) (2.50 g, 3.47 mmol) in acetonitrile (25 ml) and water (1.5 ml) at 50° C. The resulting clear solution was cooled to RT over 30 mins. Crystallisation started to occur at an internal temperature of ˜30° C. The resulting slurry was stirred for at RT for 16 h, The crystals were collected by filtration, and the filter cake washed with acetonitrile/water (95:5) and dried at 50° C. under vacuum to afford the title compound;

Quelle