HRID703822
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Methyl [2-[(methylamino)carbonyl]-1-(3-propylphenyl)hydrazino]acetate (0.5 g) was dissolved in methanol (20 ml) under nitrogen at room temperature. Solid sodium methoxide (0.24 g) was added to the solution which was then stirred at room temperature for 1 h. The reaction mixture was poured into pH 6.5 phosphate buffer solution (10 ml) and extracted with ethyl acetate (3×30 ml). The combined, dried organic phases were concentrated in vacuo and the residual oil was purified by FCC eluting with chloroform:ether (95:5) to give a solid (152 mg) which was triturated with ether to give the title compound (90 mg), m.p. 112°-115°.
WORKUP
后处理
- extractionextracted with ethyl acetate (3×30 ml)
- concentrationdried organic phases were concentrated in vacuo
- customthe residual oil was purified by FCC
- washeluting with chloroform:ether (95:5)