HRID2222234

反应详情

EQUATION

反应方程式

HRID 2222234 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

To a solution of 5-[2-[(6-chloroquinolin-4-yl)methyl]-7-(cyclopropylmethyl)-6-oxo-4-thioxo-4,5,6,7-tetrahydro-2H-pyrazolo[3,4-d]pyrimidin-3-yl]-1-methyl-1H-pyrrole-3-carbonitrile (0.24 g) in THF (5 mL) were added hydrazine hydrate (0.30 mL) and mercury chloride (0.30 g). After 4 h, a second addition of hydrazine hydrate (0.20 mL) and mercury chloride (0.30 g) was done. After stirring overnight, the mixture was diluted with water and ethyl acetate. The mixture was then filtered through a celite bed. The organic solution was collected, washed with saturated NaHCO3 and brine, dried (Na2SO4), filtered and concentrated. The residue was purified by flash chromatography using a FlashMaster™ yielding 0.18 g.

WORKUP

后处理

  1. filtrationThe mixture was then filtered through a celite bed
  2. customThe organic solution was collected
  3. washwashed with saturated NaHCO3 and brine
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue was purified by flash chromatography
  8. customyielding 0.18 g