HRID451461

反应详情

EQUATION

反应方程式

HRID 451461 的结构方程式

PROCEDURE

实验过程

1-(3-Methyl-1,2,4-thiadiazol-5-yl)piperidin-4-amine dihydrochloride (see example 36b, 2.3 g, 8.48 mmol) was neutralized with 2 N NaOH solution, The water layer was extracted three times with CH2Cl2 and three times with ethyl acetate, the combined organic phases were dried over Na2SO4, filtered and the solvents were evaporated. The crude product was purified by flash chromatography with CH2Cl2 and MeOH over a 50 g Si—NH2 column. The title compound was isolated as a light yellow oil (1.2 g, 71%).

WORKUP

后处理

  1. extractionThe water layer was extracted three times with CH2Cl2 and three times with ethyl acetate
  2. dry with materialthe combined organic phases were dried over Na2SO4
  3. filtrationfiltered
  4. customthe solvents were evaporated
  5. customThe crude product was purified by flash chromatography with CH2Cl2 and MeOH over a 50 g Si—NH2 column