HRID1094799

反应详情

EQUATION

反应方程式

HRID 1094799 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1-methyl-1H-1,2,3-triazole-5-carbaldehyde (Preparation 33, 5 g, 45 mmol) and sodium hydroxide (8.59 g, 215 mmol) in water (120 ml) at 15° C. was added dropwise a solution of potassium permanganate (5.83 g, 36.9 mmol) in water (120 ml). The reaction was stirred at room temperature for 30 minutes and then heated to reflux for 1 hour. The reaction was filtered and the filtrate acidified to pH 3 with concentrated HCl before extracting with ethyl acetate (3×100 ml). The combined organic extracts were washed with saturated aqueous brine, dried over Na2SO4 and concentrated in vacuo to afford the title compound.

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for 1 hour
  3. filtrationThe reaction was filtered
  4. extractionbefore extracting with ethyl acetate (3×100 ml)
  5. washThe combined organic extracts were washed with saturated aqueous brine
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated in vacuo