HRID2113787

反应详情

EQUATION

反应方程式

HRID 2113787 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

7-(2-Chloro-4,6-dimethylphenyl)-2-methyl-3-(1-propylbut-1-enyl)-4,5,6,7-tetrahydro-2H-pyrazolo[3,4-b]pyridine (3-1; 41.5 mg) was dissolved in acetic acid (1 mL) and 12 mg of 10% palladium on carbon was added. The mixture was stirred under hydrogen at one atmosphere for 12 h. The mixture was diluted with ethyl acetate and filtered through diatomaceous earth and the residue was washed with ethyl acetate. The ethyl acetate filtrate was washed with aqueous sodium bicarbonate, dried with magnesium sulfate, and concentrated. The residue was chromatographed on silica gel eluting with an acetone/hexane gradient to provide 10.2 mg of 4-1 as a crystalline film: ms (MH+)=374.

WORKUP

后处理

  1. filtrationfiltered through diatomaceous earth
  2. washthe residue was washed with ethyl acetate
  3. washThe ethyl acetate filtrate was washed with aqueous sodium bicarbonate
  4. dry with materialdried with magnesium sulfate
  5. concentrationconcentrated
  6. customThe residue was chromatographed on silica gel eluting with an acetone/hexane gradient