HRID536027

反应详情

EQUATION

反应方程式

HRID 536027 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To the mixture of methanol (2 ml) and NaH (45 mg, 1.1 mmol), 2-Chloro-1-propyl-8-[1-(3-trifluoromethyl-benzyl)-1H-pyrazol-4-yl]-1,7-dihydro-purin-6-one (50 mg, 0.11 mmol) was added and refluxed for 2 hours at 80° C. Reaction mixture was cooled, diluted with ethyl acetate (10 ml) and quenched with saturated NH4Cl solution. The organic layer was separated and washed with brine (2×10 ml), dried over Na2SO4, filtered and evaporated. The residue obtained was purified by preparative HPLC to obtain pure 2-Methoxy-1-propyl-8-[1-(3-trifluoromethyl-benzyl)-1H-pyrazol-4-yl]-1,7-dihydro-purin-6-one (26 mg, 53%) as an off white solid.

WORKUP

后处理

  1. additionwas added
  2. customReaction mixture
  3. temperaturewas cooled
  4. customquenched with saturated NH4Cl solution
  5. customThe organic layer was separated
  6. washwashed with brine (2×10 ml)
  7. dry with materialdried over Na2SO4
  8. filtrationfiltered
  9. customevaporated
  10. customThe residue obtained
  11. customwas purified by preparative HPLC