Methylhydrazine → HCID 44480524, compound

Participants

Reaction Steps

101 g (198.7 mmol) of ethyl (4R)-6-(bromomethyl)-4-(4-cyanophenyl)-2-oxo-1-[3-(trifluoromethyl)phenyl]-1,2,3,4-tetrahydropyrimidine-5-carboxylate (Example 6A) were initially charged in 2400 ml of dioxane. 27.46 g (596.1 mmol) of methylhydrazine were added dropwise to the solution, and the reaction mixture was then stirred at boiling point for 3 h. The mixture was then concentrated, and the residue was dissolved in dichloromethane and washed with water. The organic phase was dried over sodium sulphate and concentrated. The residue that remained was chomatographed on silica gel (mobile phase: dichloromethane/methanol 95:5). The solid which was obtained after concentration of the product fractions was triturated with diethyl ether, filtered off with suction and then dried at 50° C. under reduced pressure for 4 days. This gave 56.8 g (66% of theory) of the title compound.

Provenance & Evidence