反应详情

温度

80 °C

A solution of ethyl 6-methyl-2-(trifluoromethyl)pyrimidine-4-carboxylate (2.00 g, 8.54 mmol, prepared as described in WO2007/090748) in acetic acid (12 mL) was treated with bromine (1.36 g, 8.54 mmol) and the reaction was heated to 80° C. in a sealed vial for 30 minutes, at which time, the color of bromine was dissipated. The acetic acid was removed in vacuo and was followed by dissolving of the residue in toluene and removal of solvent in vacuo. The percent by weight of desired component in the mixture (containing unreacted starting material and overbrominated product) was determined by NMR and the mixture used without further purification (1.62 g, 61%). 1H NMR (300 MHz, CDCl3): δ 8.32 (s, 1H), 4.60 (s, 2H), 4.54 (q, 2H), 1.46 (t, 3H); LCMS (M+H)+: 313.0, 315.0

1. customThe acetic acid was removed in vacuo
2. dissolutionby dissolving of the residue in toluene
3. customremoval of solvent in vacuo
4. additionThe percent by weight of desired component in the mixture (containing unreacted starting material and overbrominated product)
5. customthe mixture used without further purification (1.62 g, 61%)