Dimethylamine → HCID 56626169, compound

Participants

Reaction Steps

13.6 g (0.3 mole) of dimethylamine were introduced into a mixture of 350 ml of isopropanol and 12 g of glacial acetic acid, while cooling with ice. 21.8 g (0.1 mole) of 4-amino-6-fluoro-tert.-butyl-3-methylthio-1,2,4-triazin-5-one (obtained as described in Example 2) were then added to this reaction solution. The mixture was allowed to warm to room temperature and was then heated under reflux for 15 hours. Thereafter, the reaction mixture was concentrated and the oily residue was stirred into water. The mixture was extracted with methylene chloride and the extract was dried over sodium sulphate and concentrated. The oily residue was taken up in diisopropyl ether, seed crystals were added and the solid which crystallized out was filtered off and dried. 15.9 g (69% of theory) of 4-amino-3-dimethylamino-6-fluoro-tert.-butyl-1,2,4-triazin-5-one of melting point 86°-87° C. were obtained.

Provenance & Evidence