HRID449061
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe dioxane was removed in vacuo
- additionDCM was added
- extractionto extract the product
- dry with materialdried (Na2SO4)
- customremoved under reduced pressure
- customto give a residue which
- customwas then purified by flash chromatography (5% MeOH in DCM)
- customHPLC: tR=2.23 min (polar—5 min)