HRID1010971

反应详情

EQUATION

反应方程式

HRID 1010971 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of 2-[(1-methylbutyl)oxy]-8-methoxy-9H-purin-6-amine trifluoroacetic acid salt (218 mg) in dry DMF (3.71 mL) was added potassium carbonate (330 mg). The mixture was stirred at 60° C. for 90 mins. The reaction was cooled and 4-(bromomethyl)tetrahydro-2H-pyran (118 mg) was added. The reaction was stirred at 50° C. for 6 h and was cooled to room temperature. The mixture was taken up in EtOAc (40 mL) and washed with water (2×20 mL). The organics were separated, dried over MgSO4 and concentrated in vacuo to give a viscous yellow oil. The material was purified by C18 reverse phase chromatography (ISCO) using water (0.1% formic acid)-acetonitrile (0.05% formic acid) as eluent (20-60%) to afford the title compound as a clear oil (92 mg).

WORKUP

后处理

  1. temperatureThe reaction was cooled
  2. stirringThe reaction was stirred at 50° C. for 6 h
  3. temperaturewas cooled to room temperature
  4. washwashed with water (2×20 mL)
  5. customThe organics were separated
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated in vacuo
  8. customto give a viscous yellow oil
  9. customThe material was purified by C18 reverse phase chromatography (ISCO)