反应详情

A mixture of 12.6 parts of 1-(phenylmethyl)-4-piperidinol, 3.2 parts of a sodium hydride dispersion 50% and 200 parts of N,N-dimethylacetamide was stirred for 1 hour at room temperature. 18 Parts of 9-[(4-fluorophenyl)methyl]-8-(methylthio)-9H-purine were added portionwise and upon completion, stirring was continued for 4 hours at room temperature. The reaction mixture was poured into water. The product was filtered off and taken up in trichloromethane. The organic layer was washed with water and filtered over diatomaceous earth. The filtrate was dried, filtered and evaporated. After crystallization from acetonitrile, the product was filtered off and dried, yielding 16.75 parts (61.1%) of 9-[(4-fluorophenyl)methyl]-8-[[1-(phenylmethyl)-4-piperidinyl]oxy]-9H-purine; mp. 117.0° C. (compound 5).

1. stirringstirring
2. waitwas continued for 4 hours at room temperature
3. filtrationThe product was filtered off
4. washThe organic layer was washed with water
5. filtrationfiltered over diatomaceous earth
6. customThe filtrate was dried
7. filtrationfiltered
8. customevaporated
9. customAfter crystallization from acetonitrile
10. filtrationthe product was filtered off
11. customdried