HRID352105
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 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
- customThe solvent was removed in vacuo
- dissolutionthe residue dissolved in water
- extractionextracted with ethyl acetate (three times)
- washThe combined organic extracts were washed with water
- dry with materialdried (magnesium sulphate)
- customevaporated
- customto give an oil
- customThe solvent was removed in vacuo
- customthe residue triturated with ethyl acetate
- customThe solid was collected
- customdried