Methanol → HCID 67581816, compound

Participants

Reaction Conditions

Reaction Steps

A suspension of 208.4 g (0.8 mol) of 2-chloro-5-fluoro-4-morpholinonitrobenzene in 516.6 g (0.88 mol) of tri(methyltetraethoxy)amine and 105 g of methanol, together with 18 g of a palladium/activated carbon catalyst (5% by weight of palladium, 50% water-moist) is introduced, at room temperature into a 2000 ml autoclave fitted with gas-dispersion stirrer. The autoclave is closed and rendered inert using nitrogen, and the mixture is reacted at a reaction temperature of from 80 to 100° C. at a hydrogen pressure of from 5 to 30 bar until no more hydrogen is absorbed. After the catalyst has been filtered off with suction, 57.5 g (0.72 mol) of 50% strength NaOH are added to the reaction solution at room temperature, followed by 161.6 g (0.9 mol) of benzyl chloroformate (95% strength). When the addition is complete, the mixture is stirred for a further 15 minutes at 50° C., and 775 g of water and 36 g (0.9 mol) of NaOH are added to the reaction solution/suspension. The solid formed is filtered off with suction, washed with water and then recrystallized from methanol.

Provenance & Evidence