2-chloro-N-(phenylmethyl)-9-(tetrahydro-3-thienyl)-9H-purin-6-amine → N2-(4-amino-cyclohexyl)-N6-(phenylmethyl)-9-(tetrahydro-3-thienyl)-9H-purine-2,6-diamine Dihydrochloride

Participants

Reaction Steps

400 mg of trans-1,4-diaminocyclohexane is taken to a temperature of 60 to 70° C., then 119 mg of the product obtained in Stage 2 above is added and the reaction medium is taken to a temperature of 130 to 140° C. for 3 hours, then left to return to ambient temperature, 5 ml of water is added followed by extracting with 3×10 ml of ethyl acetate, washing with 10 ml of water and 5 ml of an aqueous solution of sodium chloride, drying and evaporating to dryness. After purification on silica eluting with methanol/ammonium hydroxide (NH4OH) in a proportion of 98/2, followed by salification with 1.4N hydrochloric acid in ethanol, leaving to crystallize for 2 days at ambient temperature, separating, washing with 10 ml of ethanol and drying at a temperature of approximately 50° C. In this way 112 mg of expected product is obtained in the form of crystals white/cream.

Provenance & Evidence