Formaldehyde → HCID 20322577, compound

Participants

Reaction Steps

To 5.5 g of the 7,9-diethyl-3,6,7,9-tetramethyl-1,3,8-triazaspiro[4.5]decane-2,4-dione (Compound 2) obtained in Example 2 were added 1.8 g of formic acid and 6.3 g of 37% formalin; the mixture was stirred at room temperature for one hour and then refluxed by heating for 5 hours. After cooling the reaction mixture, its pH was adjusted to a value of 8 by addition of a 5% aqueous solution of sodium hydrogen carbonate; the solution was then extracted with ethyl acetate. The extract was dried over potassium carbonate and the solvent was then removed. The residue was purified by column chromatography on silica gel (eluent: ethyl acetate) to give 5.58 g of Compound 64, mp 190° - 195° C.

Provenance & Evidence