HRID1011185

反应详情

EQUATION

反应方程式

HRID 1011185 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

8-Bromo-2-[(2-methylpropyl)oxy]-9-(tetrahydro-2H-pyran-4-ylmethyl)-9H-purin-6-amine (100 mg) in n-butanol (2 mL) was refluxed with concentrated hydrochloric acid (2 mL) at 100° C. (external temperature) for 3 hours. The reaction mixture was evaporated under reduced pressure to dryness. To the reaction mixture was then added a small volume of water and an equivalent volume of methanol to give a suspension, which was then neutralised to by the addition of 2M sodium hydroxide (from pH ˜3 to 7). This was then evaporated under reduced pressure to give a beige solid which was purified by C18 reverse phase chromatography using water (containing 0.1% formic acid)-acetonitrile (containing 0.05% formic acid) as eluent (20-60%). This gave the title compound (13 mg) as white solid.

WORKUP

后处理

  1. customThe reaction mixture was evaporated under reduced pressure to dryness
  2. additionTo the reaction mixture was then added a small volume of water
  3. customan equivalent volume of methanol to give a suspension, which
  4. customThis was then evaporated under reduced pressure
  5. customto give a beige solid which
  6. customwas purified by C18 reverse phase chromatography