反应详情

2.5 g 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 (may be prepared as in Preparation 1; 3.47 mmol) were dissolved in 25 mL acetonitrile and 1.5 mL water at 50° C. 409 mg succinic acid (3.47 mmol) was added. The acid dissolved immediately and the clear solution was cooled down to room temperature over 30 minutes. At approximately 30° C. the crystallization took place. The slurry was then stirred for approximately 16 h at room temperature. The crystals were collected by filtration. The filter cake was washed in portions with 9 ml acetonitrile/water 95:5 v/v and dried for 16 h at 50° C. and at around 10 mbar.

1. customat 50° C
2. dissolutionThe acid dissolved immediately
3. customAt approximately 30° C. the crystallization
4. filtrationThe crystals were collected by filtration
5. washThe filter cake was washed in portions with 9 ml acetonitrile/water 95:5 v/v
6. customdried for 16 h at 50° C. and at around 10 mbar