HRID1945221

反应详情

EQUATION

反应方程式

HRID 1945221 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Sodium hydride (60% disp. oil, 0.024 g) was added to the product from step (iv) (0.20 g) in dry DMF (10 ml) and stirred at RT for 30 min before adding methyl-bromoacetate (0.060 ml). The solution was stirred at RT for 2 h, diluted with water and extracted with diethylether. The organics were dried and evaporated under reduced pressure to give an oil. The oil was dissolved in THF (20 ml) and water (10 ml) then sodium hydroxide (0.037 g) was added and stirred at RT overnight. The mixture was acidified with 2M HCl, extracted with ethyl acetate, the organics dried and evaporated under reduced pressure. The residue was purified by reverse phase HPLC. Yield 0.045 g

WORKUP

后处理

  1. stirringThe solution was stirred at RT for 2 h
  2. extractionextracted with diethylether
  3. customThe organics were dried
  4. customevaporated under reduced pressure
  5. customto give an oil
  6. stirringstirred at RT overnight
  7. extractionextracted with ethyl acetate
  8. customthe organics dried
  9. customevaporated under reduced pressure
  10. customThe residue was purified by reverse phase HPLC