HRID896054

反应详情

EQUATION

反应方程式

HRID 896054 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1-(3-Dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (0.201 g, 1.30 mmol) is added to 5,6-diamino-1-isobutyl-3-methyl-1H-pyrimidine-2,4-dione (0.223 g, 1.05 mmol)) and (6,7-dimethoxy-1-methyl-isoquinolin4-yl)-acetic acid (0.25 g, 0.96 mmol) in methanol (5 ml) and water (1 ml) and the mixture is stirred at ambient temperature for 16 hours. The methanol is evaporated and the resultant solid collected by filtration, taken into methanol (5 ml) and 5M aqueous sodium hydroxide (0.5 ml) is added. The reaction is heated to reflux for 1 hour, cooled to ambient temperature and evaporated. The residue is dissolved in water and extracted with dichloromethane, the combined organic extracts are dried over sodium sulfate and evaporated to afford 8-(6,7-dimethoxy-1-methyl-isoquinolin4-ylmethyl)-3-isobutyl-1-methyl-3,7-dihydro-purine-2,6-dione, M+ 437.

WORKUP

后处理

  1. customThe methanol is evaporated
  2. filtrationthe resultant solid collected by filtration
  3. additionis added
  4. temperatureThe reaction is heated
  5. temperatureto reflux for 1 hour
  6. temperaturecooled to ambient temperature
  7. customevaporated
  8. dissolutionThe residue is dissolved in water
  9. extractionextracted with dichloromethane
  10. dry with materialthe combined organic extracts are dried over sodium sulfate
  11. customevaporated