Methylhydrazine → HCID 44480784, compound

Participants

Reaction Steps

Under an atmosphere of argon protective gas, ethyl 6-(bromomethyl)-4-[4-cyano-2-(trifluoro-methyl)phenyl]-2-oxo-1-[3-(trifluoromethyl)phenyl]-1,2,3,4-tetrahydropyrimidine-5-carboxylate (576 mg, 1 mmol; Example 21A) was initially charged in dioxane (20 ml). Methylhydrazine (128 mg, 3 mmol) was added dropwise to the reaction mixture, and the mixture was then stirred at boiling point for 8 h (bath temperature 120° C.). The reaction mixture was then concentrated, and the residue was purified by preparative HPLC (column: Gromsil C18 10 μm; mobile phase: acetonitrile/water+0.1% TFA 10:90→90:10). This gave the target compound as a solid which was reprecipitated from acetonitrile/water (Yield: 205 mg, 41% of theory).

Provenance & Evidence