HRID1293025

反应详情

EQUATION

反应方程式

HRID 1293025 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-Naphthylmethanamine (5.4 g, 19.7 mmol) was added to a stirred solution of 2,6-dichloro-9-(tetrahydro-2H-pyran-2-yl)-9H-purine (3.5 g, 22.3 mmol) (Preparation 19) and triethylamine (4 g, 39.6 mmol) in acetonitrile (150 ml) at room temperature. The reaction mixture was stirred at room temperature for 64 hours. The solvent was removed under reduced pressure, ethyl acetate (100 ml) was added and then the solvent was removed under reduced pressure again. The residue was purified by column chromatography on silica gel eluting with pentane: ethyl acetate (1:1 by volume) increasing in polarity to neat ethyl acetate. The solvent was removed under reduced pressure to give the title compound (7.56 g) as a solid.

WORKUP

后处理

  1. customThe solvent was removed under reduced pressure, ethyl acetate (100 ml)
  2. additionwas added
  3. customthe solvent was removed under reduced pressure again
  4. customThe residue was purified by column chromatography on silica gel eluting with pentane: ethyl acetate (1:1 by volume)
  5. temperatureincreasing in polarity to neat ethyl acetate
  6. customThe solvent was removed under reduced pressure