反应详情

A solution of 2-Bromo-N-pyrimidin-4-yl-acetamide (0.90 g, 4.17 mmol) and hydroxy-di-thiophen-2-yl-acetic acid (R)-(1-aza-bicyclo[2.2.2]oct-3-yl) ester (Example 70(ii)) (1.32 g, 3.79 mmol) in dry chloroform-acetonitrile (20 ml+4 ml) are heated at 50° C. for 3 hours. The mixture is then cooled to room temperature and concentrated. Purification by reverse phase C18 column chromatography (gradient elution 100% water to 100% acetonitrile) gives after concentration a light brown solid. The solid was triturated with hot acetonitrile then dissolved in hot acetonitrile containing a few drops of water. After standing at 5° C. for several hours crystals are formed which are filtered and dried to give the title compound.

1. concentrationconcentrated
2. customPurification
3. washby reverse phase C18 column chromatography (gradient elution 100% water to 100% acetonitrile)
4. customgives
5. concentrationafter concentration a light brown solid
6. customThe solid was triturated with hot acetonitrile
7. dissolutionthen dissolved in hot acetonitrile containing a few drops of water
8. waitAfter standing at 5° C. for several hours
9. customcrystals are formed which
10. filtrationare filtered
11. customdried