Hexamethylenetetramine → HCID 20337667, compound

Participants

Reaction Steps

88 g of p-tetradecyloxy-ω-bromoacetophenone (stage 2 of compound 29) are dissolved in 320 ml of dried chloroform. 30.4 g of urotropin are added at room temperature. The solution undergoes spontaneous heating. It is stirred for 2 hours at room temperature. The chloroform is distilled off and the solid residue is rubbed with acetone. The crystalline deposit is filtered off under suction and washed repeatedly with acetone. The crude product is then introduced into a solution of 140 ml of concentrated sulphuric acid in 100 ml of ethanol, followed by stirring for 24 hours at room temperature. After filtration under suction, the residue is washed with a mixture of ethanol and concentrated hydrochloric acid (7:1), giving 80 g=95% of p-tetradecyloxy-ω-aminoacetophenone hydrochloride melting at 190°-195° C.

Provenance & Evidence