HRID1087972
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
The t-butyl ester from Example 1 (571 mg, 0.783 mmol) was dissolved in a mixture of trifluoroacetic acid (2 ml) and dichloromethane (1 ml). The solution was kept at 4° C. overnight, then concentrated to dryness under vacuum, and the residue was azeotroped six times with dichloromethane. The resulting crude product was then taken up in ethyl acetate and washed with water until the washings were neutral. The organic phase was dried (MgSO4) and evaporated under vacuum to afford the title compound (442 mg, 84%) as a white foam. Found: C,61.89; H,7.76; N,7.93. C35H52N4O9 (0.5 H2O) requires C,61.65; H,7.69; N,8.22%.
WORKUP
后处理
- concentrationconcentrated to dryness under vacuum
- customthe residue was azeotroped six times with dichloromethane
- washwashed with water until the washings
- dry with materialThe organic phase was dried (MgSO4)
- customevaporated under vacuum