反应详情

A solution of 0.2 g (0.75 mmol) of 5-amino-8,9-difluoro-3-methyl-2,3-dihydro-1-oxa-3a,5-diazaphenalene-4,6-dione (Example 24h), 0.58 g (2.0 mmol) of (S)-3-pyrrolidinylcarbamic acid tert-butyl ester (J. Med. Chem., 1992; 35:1764), 0.5 g (0.5 mmol) of triethylamine and 20 mL of acetonitrile is heated at reflux for 18 hours. The solvent is removed in vacuo and the residue is partitioned between dichloromethane-water. The organic layer is washed with water, dried (MgSO4) and concentrated in vacuo. The residue is chromatographed over flash grade silica gel (230-400 mesh) eluting with dichloromethane/ethanol (95:5) to give 0.34 g of the title compound, mp 114-116° C.

1. temperatureat reflux for 18 hours
2. customThe solvent is removed in vacuo
3. customthe residue is partitioned between dichloromethane-water
4. washThe organic layer is washed with water
5. dry with materialdried (MgSO4)
6. concentrationconcentrated in vacuo
7. customThe residue is chromatographed over flash grade silica gel (230-400 mesh)
8. washeluting with dichloromethane/ethanol (95:5)