3,5,6-Trichloro-1,2,4-triazine synthesis

Yield:873-41-6 78%

Reaction Conditions:

with phosphorus pentachloride;N,N-diethylaniline;trichlorophosphate at 120; for 5 h;

Steps:

A7.b

b) Preparation of intermediate 17; To 18 g (93.75 mmoles) of 5-bromo-6-azauracil (intermediate 16) in 150 ml of phosphorus oxychloride were added 39.2g (188 mmoles) of phosphorus pentachloride and 38 ml ( 240 mmoles) of Nv/V-diethylaniline. The mixture was stirred at 120°C for 5hours after which period the excess of solvent was evaporated. The residue was several times extracted with carbon tetrachloride. After evaporation of the solvent, the remaining oily residue was put in the refrigerator where it solidified. Yield : 13g (78%) of intermediate 17 (3,5,6-trichloro[l,2,4]triazine) (mp. 57-60°C).

References:

WO2006/15985,2006,A1 Location in patent:Page/Page column 62-63