反应详情

温度

140 °C

A mixture of [1-(2,6-dichloro-5-methoxy-pyrimidin-4-yloxy)-cyclopropyl]-methanol (800 mg, 3.02 mmol) and lithium chloride (600 mg, 14.15 mmol) in anhydrous DMF (3 mL) was heated at 140° C. for 10 minutes using microwave irradiation, then concentrated in vacuo. The resulting residue was purified by column chromatography (SiO2, gradient 0-5% methanol in DCM) affording 2,4-Dichloro-6-(1-hydroxymethyl-cyclopropoxy)-pyrimidin-5-ol (300 mg, 40%). LCMS: RT=2.52 min, [M−H]−=249/251/253.

1. custommicrowave irradiation
2. concentrationconcentrated in vacuo
3. customThe resulting residue was purified by column chromatography (SiO2, gradient 0-5% methanol in DCM)