Lithium Chloride → 2,4-Dichloro-6-(1-hydroxymethyl-cyclopropoxy)-pyrimidin-5-ol
反応式
[Cl:1][C:2]1[N:7]=[C:6]([O:8][C:9]2([CH2:12][OH:13])[CH2:11][CH2:10]2)[C:5]([O:14]C)=[C:4]([Cl:16])[N:3]=1.[Cl-].[Li+]>CN(C=O)C>[Cl:1][C:2]1[N:3]=[C:4]([Cl:16])[C:5]([OH:14])=[C:6]([O:8][C:9]2([CH2:12][OH:13])[CH2:10][CH2:11]2)[N:7]=1参加物
4
反応条件
- 温度
- 140 °C
実験手順
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.