反应详情

A mixture of 1-(4-piperidinyl)-1H-indole (4.1 g), 6-(2-chloroethyl)-7-methyl-5H-thiazolo[3,2-a]pyrimidin-5-one (3.4 g), prepared as described in EP-A-0,196,132, sodium carbonate (6 g) and potassium iodide (0.1 g) in 4-methyl-2-pentanone (250 ml) was stirred and refluxed overnight. The warm reaction mixture was filtered and the filtrate was evaporated. The residue was purified over silica gel on a glass filter (eluent: CH2Cl2 /C2H5OH 90/10). The pure fractions were collected and the solvent was evaporated. The residue was crystallized from DIPE with a small amount of CH3CN. The precipitate was filtered off and dried, yielding 3 g (51%) 6-[2-[4-(1H-indol-1-yl)-1-piperidinyl]ethyl]-7-methyl-5H-thiazolo[3,2-a]pyrimidin-5-one (compound 3; mp. 134.4° C.).

1. customprepared
2. temperaturerefluxed overnight
3. customThe warm reaction mixture
4. filtrationwas filtered
5. customthe filtrate was evaporated
6. customThe residue was purified over silica gel on a glass
7. filtrationfilter (eluent: CH2Cl2 /C2H5OH 90/10)
8. customThe pure fractions were collected
9. customthe solvent was evaporated
10. customThe residue was crystallized from DIPE with a small amount of CH3CN
11. filtrationThe precipitate was filtered off
12. customdried