Triethylamine → HCID 20306069, compound

Participants

Reaction Steps

505 g (1.5 moles) of 1-(4-biphenylyloxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-ol (A form) and 140 g (1.6 moles) of methoxymethyl isocyanate were heated under reflux in 2.5 liters of tetrahydrofuran in the presence of 40 ml of triethylamine and 1 ml of dibutyl-tin dilaurate for 48 hours. Thereafter, the solvent was stripped off in vacuo and 3 liters of petroleum ether were added to the residue. The crystalline precipitate formed was extracted by stirring with 1.5 liters of diisopropyl ether. 528 g (82.5% of theory) of 1-(4-biphenylyloxy)-3,3-dimethyl-2-methoxymethylcarbamoyloxy-1-(1,2,4-triazol-1-yl)-butane (A form) of melting point 95°-98° C. were obtained.

Provenance & Evidence