HRID1532112

反应详情

EQUATION

反应方程式

HRID 1532112 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-(2-allyloxybenzamido)-1-methyl-3-n-propylpyrazole-5-carboxamide (1.2 g, 0.0035 mol), sodium hydroxide (0.70 g, 0.018 mol), water (34 ml) and ethanol (8 ml) was refluxed for 5 hours. After cooling, the solution was exhaustively extracted with ethyl acetate. The combined extracts were washed with brine (30 ml), dried (Na2SO4), filtered and the solvent evaporated under vacuum to give a crude product which was crystallised from ethyl acetate/hexane to afford the title compound (0.476 g, 37%), m.p. 116-119° C. Found: C, 67.00; H, 6.21; N, 17.23. C18H20N4O2 requires C, 66.65; H, 6.21; N, 17.27%.

WORKUP

后处理

  1. temperaturewas refluxed for 5 hours
  2. temperatureAfter cooling
  3. extractionthe solution was exhaustively extracted with ethyl acetate
  4. washThe combined extracts were washed with brine (30 ml)
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. customthe solvent evaporated under vacuum
  8. customto give a crude product which
  9. customwas crystallised from ethyl acetate/hexane