HRID1369385

反应详情

EQUATION

反应方程式

HRID 1369385 的结构方程式

CONDITIONS

反应条件

温度
2.5 °C

PROCEDURE

实验过程

Thionyl chloride (1.2 ml) was added dropwise into a mixture of 1.41 g of 4-[6-amino-8-(3-fluorophenyl)-2-iodo-9H-9-purinyl]butanoic acid and 75 ml of methanol over 15 minutes during the mixture was stirred at 0-5° C. in a nitrogen stream. This was raised to room temperature and stirred for 45 minutes and the solvent was evaporated. The resulting residue was dissolved in ethyl acetate and then the solution was washed with a saturated aqueous solution of sodium bicarbonate twice and then with brine once. The organic layer was dried over anhydrous sodium sulfate and concentrated to give 1.45 g of the title compound. The yield was 100%.

WORKUP

后处理

  1. temperatureThis was raised to room temperature
  2. stirringstirred for 45 minutes
  3. customthe solvent was evaporated
  4. dissolutionThe resulting residue was dissolved in ethyl acetate
  5. washthe solution was washed with a saturated aqueous solution of sodium bicarbonate twice
  6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  7. concentrationconcentrated