反应详情

The product is prepared according to the procedure described in example 5, using 177 mg of sodium [4-(morpholin-4-yl)-6-oxo-1,6-dihydropyrimidin-2-yl]acetate, 236 mg of 3,3-dimethylindoline (which can be prepared according to T. W. Ramsay et al., Synth. Commun. 1995, 25, 4029) and 169 mg of N-[3-(dimethylamino)propyl]-N′-ethylcarbodiimide hydrochloride in a mixture of 0.11 ml of pyridine and 5 ml of N,N-dimethylformamide. The reaction mixture is stirred for 15 h at ambient temperature and then concentrated to dryness under reduced pressure. 40 ml of water are added to the residue and triturated with a spatula at ambient temperature. The precipitate formed is filtered off, and then solubilized with a dichloromethanemethanol mixture and dried. After concentration to dryness under reduced pressure, the crude product is purified by chromatography on a 30 g silica (0.02-0.045 mm) column, eluent: 90/10 v/v dichloromethanemethanol. After the various fractions have been evaporated, the pink solid residue is triturated from 10 ml of diisopropyl ether, filtered off, and then dried under a bell jar (1h40° C./20 mbar). 134 mg of 2-[2-(3,3-dimethyl-2,3-dihydroindol-1-yl)-2-oxoethyl]-6-morpholin-4-yl-3H-pyrimidin-4-one are thus obtained in the form of a pink solid, the characteristics of which are the following:

1. customThe product is prepared
2. concentrationconcentrated to dryness under reduced pressure
3. addition40 ml of water are added to the residue
4. customtriturated with a spatula at ambient temperature
5. customThe precipitate formed
6. filtrationis filtered off
7. customdried
8. concentrationAfter concentration to dryness under reduced pressure
9. customthe crude product is purified by chromatography on a 30 g silica (0.02-0.045 mm) column, eluent
10. customAfter the various fractions have been evaporated
11. customthe pink solid residue is triturated from 10 ml of diisopropyl ether
12. filtrationfiltered off
13. customdried under a bell jar (1h40° C./20 mbar)