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)