HRID29513

反应详情

EQUATION

反应方程式

HRID 29513 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To 51 mg (0.19 mmol) of (5-Chloro-2-nitro-phenyl)-(1-methyl-[1,2,3]triazol4-yl)-methanone in 2 ml of methanol were added 0.05 ml of 12M HCl and 200 mg (0.89 mmol) of stannous (II) chloride monohydrate, and the mixture was heated at 100° C. for four hours. The mixture was then cooled to ambient temperature, partitioned between 1M NaOH and ethyl acetate, and the phases were separated. The ethyl acetate phase was washed once each with water and brine, dried over Na2SO4, filtered, and concentrated in vacuo to a solid. The solid was chromatographed to give the title product as a yellow solid.

WORKUP

后处理

  1. temperatureThe mixture was then cooled to ambient temperature
  2. custompartitioned between 1M NaOH and ethyl acetate
  3. customthe phases were separated
  4. washThe ethyl acetate phase was washed once each with water and brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo to a solid
  8. customThe solid was chromatographed