HRID703822

反应详情

EQUATION

反应方程式

HRID 703822 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. extractionextracted with ethyl acetate (3×30 ml)
  2. concentrationdried organic phases were concentrated in vacuo
  3. customthe residual oil was purified by FCC
  4. washeluting with chloroform:ether (95:5)