HRID352105

反应详情

EQUATION

反应方程式

HRID 352105 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of the product from step (c) (286 mg) in 40% aqueous methylamine (1 ml) and tetrahydrofuran (10 ml) was stirred for 6 h. The solvent was removed in vacuo and the residue dissolved in water and extracted with ethyl acetate (three times). The combined organic extracts were washed with water, dried (magnesium sulphate) and evaporated to give an oil. To a solution of this amine in methanol (10 ml) was added a solution of oxalic acid (57 mg) in methanol. The solvent was removed in vacuo and the residue triturated with ethyl acetate. The solid was collected and dried to afford the title compound as a white solid (110 mg). M.p. 167-169° C.

WORKUP

后处理

  1. customThe solvent was removed in vacuo
  2. dissolutionthe residue dissolved in water
  3. extractionextracted with ethyl acetate (three times)
  4. washThe combined organic extracts were washed with water
  5. dry with materialdried (magnesium sulphate)
  6. customevaporated
  7. customto give an oil
  8. customThe solvent was removed in vacuo
  9. customthe residue triturated with ethyl acetate
  10. customThe solid was collected
  11. customdried