HRID257141

反应详情

EQUATION

反应方程式

HRID 257141 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a hydrogenation vessel, a solution of 14.5 g of 7-cyanobenzo-1,2,3-thiadiazole in 150 ml of methanol is treated with 4.4 g of Raney nickel and with 15 g of liquid nitrogen. Hydrogen is subsequently injected, the vessel is heated, and the mixture is hydrogenated at 60° C. and constant hydrogen pressure of 107Pa until hydrogen is no longer taken up. The mixture is then cooled, the catalyst is removed by filtration, the filtrate is evaporated and chromatographed on silica gel (hexane/ethyl acetate 2:1), resulting in the title compound of m.p. 136°-139° C.).

WORKUP

后处理

  1. temperaturethe vessel is heated
  2. customis hydrogenated at 60° C.
  3. temperatureThe mixture is then cooled
  4. customthe catalyst is removed by filtration
  5. customthe filtrate is evaporated
  6. customchromatographed on silica gel (hexane/ethyl acetate 2:1)