Methanol → HCID 14746212, compound

Participants

Reaction Steps

1.60 g of 2,4-bis-[N-ethyl-N-(2,2,6,6-tetramethyl-4-piperidyl)amino]-6-(2-hydroxyethoxy)-1,3,5-triazine [prepared as described in Preparation 3(B)] and 0.22 g of dimethyl succinate were dissolved in 20 ml of toluene, and a catalytic amount of tetraisopropyl titanate was added to the resulting solution. The resulting mixture was first agitated at 100° to 105° C. for 3 hours whilst the methanol generated was removed by distillation, and then the temperature was elevated to 130° C. to remove the toluene. When this removal was complete, a mixture of ethyl acetate and water was added to the residue, and then the mixture was shaken. The ethyl acetate layer was then separated, dried and concentrated by evaporation under reduced pressure, and the resulting residue was purified by silica gel column chromatography (using a 10:3:1 by volume mixture of diethyl ether, ethanol and triethylamine as eluent), to obtain 920 mg of the title compound as crystals melting at 85° C.

Provenance & Evidence