HRID1011030

反应详情

EQUATION

反应方程式

HRID 1011030 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
1 °C

PROCEDURE

实验过程

2-[(Tetrahydro-2-furanylmethyl)oxy]-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine (1.7202 g) was dissolved in chloroform (15 mL) and cooled to ˜1° C. before N-bromosuccinimide (1.056 g) was added keeping the reaction temperature below 2° C. The reaction mixture was then stirred at ˜1° C. for 30 minutes before allowing to warm to room temperature were upon the reaction mixture was stirred for 3 hours. The reaction mixture was then stood overnight at room temperature before being partitioned between water (50 mL) and the organic phase separated using a hydrophobic frit. The organic phase was evaporated under reduced pressure to give a brown gum which was purified using silica chromatography (ISCO) eluting with 0-100% ethyl acetate: cyclohexane. This gave the title compound as a white foam solid (1.3748 g).

WORKUP

后处理

  1. additionwas added
  2. customthe reaction temperature below 2° C
  3. temperatureto warm to room temperature
  4. stirringwas stirred for 3 hours
  5. waitThe reaction mixture was then stood overnight at room temperature
  6. custombefore being partitioned between water (50 mL)
  7. customthe organic phase separated
  8. customThe organic phase was evaporated under reduced pressure
  9. customto give a brown gum which
  10. customwas purified
  11. washeluting with 0-100% ethyl acetate