反应详情

温度

85 °C

2.3 g of 5-cyano-3-methyl-pyridine-2-carboxylic acid [3-((R)-5-amino-3-difluoromethyl-3,6-dihydro-2H-[1,4]oxazin-3-yl)-4-fluoro-phenyl]-amide (5.702 mml) was put in a 4neck flask. In an Erlenmeyer flask 92 ml acetonitrile and 4.6 ml water were added. The mixture was shaken for a few seconds and 561.6 mg of HCl 37% (5.702 mmol) were added. The solution was shaken again for a few seconds and then it was added to the 4neck flask in portions. The mixture was stirred with a paddle and it was heated in a water bath up to 85° C. At 85° C. all the solid material was completely dissolved and a slightly yellow clear solution was obtained. The solution was left at rt to cool down with stirring. Precipitate appeared at 40° C. The suspension was let to stir overnight and it was filtered after 16 hours through a Büchner filter. The isolated material was dried in an oven at rt for 16 h and 1854.5 mg of a white powder was obtained.

1. stirringThe solution was shaken again for a few seconds
2. additionit was added to the 4neck flask in portions
3. stirringThe mixture was stirred with a paddle and it
4. dissolutionAt 85° C. all the solid material was completely dissolved
5. customa slightly yellow clear solution was obtained
6. waitThe solution was left at rt
7. temperatureto cool down
8. stirringwith stirring
9. customappeared at 40° C
10. stirringto stir overnight
11. filtrationit was filtered after 16 hours through a Büchner
12. filtrationfilter
13. customThe isolated material was dried in an oven at rt for 16 h