反应详情

A solution of 0.12 g (0.45 mmol) of 5-amino-8,9-difluoro-5-methyl-6,7-dihydro-5H-pyrido[3,2,1-ij]quinazoline-1,3-dione (Example 24i), 0.34 g (1.8 mmol) of (S)-3-pyrrolidinylcarbamic acid tert-butyl ester (J. Med. Chem., 1992; 35:1764), 0.2 g (2.0 mmol) of triethylamine and 7 mL of dimethyl sulfoxide is heated at 110° C. for 18 hours. The reaction is cooled to room temperature, diluted with 80 mL of ice and water and stirred at 5° C. for 1 hour. The resulting precipitate is removed by filtration, washed with water and dried in vacuo. The solid is chromatographed over flash grade silica gel (230–400 mesh) eluting with dichloromethane/ethanol (9:1) to give 0.14 g of the title compound, mp 98–100° C.

1. customThe resulting precipitate is removed by filtration
2. washwashed with water
3. customdried in vacuo
4. customThe solid is chromatographed over flash grade silica gel (230–400 mesh)
5. washeluting with dichloromethane/ethanol (9:1)