Formaldehyde → HCID 20194908, compound

Participants

Reaction Steps

The hydroxymethylation of dimethyl 4,4-dimethoxybutane-1,1-dicarboxylate was carried out. The diester (23.4 g, 0.10 mol) was added dropwise to a mixture of formalin (8.1 ml, 0.10 mol) and potassium hydrogen carbonate (0.8 g, 8 mmol) over 20 min. The mixture was stirred at room temperature for 6 hours until the starting ester was completely consumed. A saturated aqueous solution of ammonium sulfate (35 ml) was added to the reaction mixture. The mixture was then extracted with three 60 ml portions of ethyl ether and the combined extracts were dried over anhydrous magnesium sulfate. The salt was filtered off and rotary evaporation of the solvent from the filtrate gave the product, at 95% yield, as viscous oil.

Provenance & Evidence