反应详情

A mixture of 22.4 parts of N-[4-[(2-ethoxyethyl)amino]-5-pyrimidinyl]-N'-[1-(phenylmethyl)-4-piperidinyl]thiourea, 17.3 parts of mercury(II) oxide, 0.1 parts of sulfur and 270 parts of tetrahydrofuran was stirred for 2 hours at reflux temperature. The reaction mixture was filtered while hot over diatomaceous earth. The filtrate was evaporated and the residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated, yielding 16.3 parts (79.3%) of 9-(2-ethoxyethyl)-N-[1-(phenylmethyl)-4-piperidinyl]-9H-purin-8-amine as a residue (compound 11).

1. temperatureat reflux temperature
2. filtrationThe reaction mixture was filtered while hot over diatomaceous earth
3. customThe filtrate was evaporated
4. customthe residue was purified by column chromatography over silica gel using
5. additiona mixture of trichloromethane and methanol (95:5 by volume) as eluent
6. customThe pure fractions were collected
7. customthe eluent was evaporated