HRID2111658

反应详情

EQUATION

反应方程式

HRID 2111658 的结构方程式

PROCEDURE

实验过程

Sodium (415 mg, 18.0 mmol) was added and completely dissolved in methanol (18 ml). Thereafter, 2-butoxy-9-(6-chloro-3-pyridylmethyl)adenine (300 mg, 0.90 mmol) was added thereto, and the resultant was heated under reflux for 24 hours. The reaction solution was concentrated under reduced pressure, water (30 ml) was added to the residue, and the resultant was neutralized with concentrated hydrochloric acid under ice cooling. The precipitated solid was collected by filtration, and crude crystal was purified by silica gel column chromatography (methylene chloride:methanol=50:1) to obtain 148 mg of the title compound (yield: 50%).

WORKUP

后处理

  1. temperaturethe resultant was heated
  2. temperatureunder reflux for 24 hours
  3. concentrationThe reaction solution was concentrated under reduced pressure, water (30 ml)
  4. additionwas added to the residue
  5. filtrationThe precipitated solid was collected by filtration
  6. customcrude crystal was purified by silica gel column chromatography (methylene chloride:methanol=50:1)