Methane → 3-Cyano-2-morpholino-5-(pyrid-4-yl)pyridine

Participants

Reaction Conditions

Reaction Steps

5.3 kg 3-cyano-2-morpholino-5-(pyrid-4-yl)-pyridine hydrochloride monohydrate is suspended in 40 l water and the suspension is heated to 50° C. 0.5 kg activated charcoal is added and filtered off with suction after 15 minutes of stirring and washed with water. The filtrate is cooled to 30° C. While stirring, about 2.7 l concentrated sodium hydroxide solution is allowed to run in over a period of one hour at this temperature until pH 8-9. The crystalline material is centrifuged off and washed with total of 30 l water. The yield is 4.1 kg (93.2% of the theoretical yield), with a melting point of 126° C.-128° C. The bulk density of the material, after is was pulverized in a mortar, was about 360 g/l.

Provenance & Evidence