HRID1922860

反应详情

EQUATION

反应方程式

HRID 1922860 的结构方程式

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 2,6-dichloro-9H-purine (2.18 g, 11.53 mmol), (R)-3-methylmorpholine (1.40 g, 13.84 mmol) and DIPEA (2.57 mL, 14.99 mmol) in IMS (50 mL) were heated at 80° C. for 8 h. The reaction mixture was concentrated in vacuo to a reduced volume and the residue partitioned between EtOAc and H2O. The organic phase was dried (Na2SO4) and concentrated in vacuo. The resulting residue was purified by column chromatography (Si—PCC, MeOH:EtOAc, 0-10%) affording the title compound as an off-white solid (914 mg, 31%). LCMS (method H): RT 2.53 min [M+H]+ 254.3

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated in vacuo to a reduced volume
  2. customthe residue partitioned between EtOAc and H2O
  3. dry with materialThe organic phase was dried (Na2SO4)
  4. concentrationconcentrated in vacuo
  5. customThe resulting residue was purified by column chromatography (Si—PCC, MeOH:EtOAc, 0-10%)