HRID1638211
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
(8-Cyclodecyl-4-oxo-1-phenyl-1,3,8-triaza-spiro[4,5]dec-3-yl)-acetic acid methyl ester (0.8 mmol) was dissolved in ethyleneglycol dimethylether (2 ml). Lithiumchloride (0.8 mmol) and sodium borohydride (0.8 mol) were added. After stirring for 4 h the reaction mixture was distributed between dichloromethane/water/methanol. The organic layer was separated, dried over magnesium sulfate and evaporated. The residue was purified by column chromatography (SiO2, ethyl acetate). Formation of the HCl-salt yielded the title compound as a white solid, 0.124 g, m. p. 190° C. and MS: m/e=414.5 (M+H+).
WORKUP
后处理
- customThe organic layer was separated
- dry with materialdried over magnesium sulfate
- customevaporated
- customThe residue was purified by column chromatography (SiO2, ethyl acetate)