反应详情

温度

130 °C

0.246 g (1 mmol) of (E)-2-[2-(3-chloro-phenyl)-vinyl]-6-methyl-pyrimidin-4-ol were treated with 1.83 ml (20 mmol) of POCl3 and subsequently heated at 130° C. for 4.5 hours. The mixture was cooled to RT, concentrated in vacuo and the residue was partitioned between EtOAc, water and saturated KHCO3. The organic layer was separated, dried over sodium sulphate and concentrated in vacuo. The residue was applied to a short silica gel column with CH2Cl2/hexane (3:2) as eluent. Combination of the purified fractions and concentration in vacuo gave 188 mg (71%) of the desired (E)-4-chloro-2-[2-(3-chloro-phenyl)-vinyl]-6-methyl-pyrimidine as a white solid. EI mass spectrum, m/e: 264 (M calculated for C13H10Cl2N2: 264)

1. temperatureThe mixture was cooled to RT
2. concentrationconcentrated in vacuo
3. customthe residue was partitioned between EtOAc, water and saturated KHCO3
4. customThe organic layer was separated
5. dry with materialdried over sodium sulphate
6. concentrationconcentrated in vacuo
7. concentrationCombination of the purified fractions and concentration in vacuo