HRID1087972

反应详情

EQUATION

反应方程式

HRID 1087972 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. concentrationconcentrated to dryness under vacuum
  2. customthe residue was azeotroped six times with dichloromethane
  3. washwashed with water until the washings
  4. dry with materialThe organic phase was dried (MgSO4)
  5. customevaporated under vacuum