HRID449061

反应详情

EQUATION

反应方程式

HRID 449061 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of trans-toluene-4-sulfonic acid 3-[8-amino-1-(4-phenoxy-phenyl)-imidazo[1,5-a]pyrazin-3-yl]-cyclobutylmethyl ester (10.0 mg, 0.0185 mmol), potassium hydroxide (10.4 mg, 0.185 mmol), H2O (1 mL) and 1,4-dioxane (1 mL) was heated to 60° C. overnight. The mixture was titrated to pH 2 with 2M HCl. The dioxane was removed in vacuo. DCM was added to extract the product. The organics were combined, dried (Na2SO4) and removed under reduced pressure to give a residue which was then purified by flash chromatography (5% MeOH in DCM). MS (ES+): m/z 386.94 (100) [MH+]. HPLC: tR=2.23 min (polar—5 min).

WORKUP

后处理

  1. customThe dioxane was removed in vacuo
  2. additionDCM was added
  3. extractionto extract the product
  4. dry with materialdried (Na2SO4)
  5. customremoved under reduced pressure
  6. customto give a residue which
  7. customwas then purified by flash chromatography (5% MeOH in DCM)
  8. customHPLC: tR=2.23 min (polar—5 min)