HRID590884

反应详情

EQUATION

反应方程式

HRID 590884 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (3-(bis(4-methoxybenzyl)amino)-1-trityl-1H-pyrazolo[4,3-c]pyridin-6-yl)carbamate (0.4 g, 0.55 mmol) in THF (8 mL) was added TBAF (1.0 M solution in THF, 10 mL) and the contents were heated to reflux. After 12 h, the reaction was cooled back to ambient temperature, quenched with 1N HCl (5 mL) and stirred at ambient temperature for 1 h. The reaction mixture was further diluted with EtOAc (25 mL) and the organic layer was separated. The organic layer was washed with brine (1×20 mL), dried over anhydrous Na2SO4 and the solvents were removed under reduced pressure. The residue thus obtained was purified by a filter column to afford the title compound. MS ES calc'd. for C41F137N5O2 [M+H]+ 632. Found 632.

WORKUP

后处理

  1. temperaturethe contents were heated to reflux
  2. customquenched with 1N HCl (5 mL)
  3. additionThe reaction mixture was further diluted with EtOAc (25 mL)
  4. customthe organic layer was separated
  5. washThe organic layer was washed with brine (1×20 mL)
  6. dry with materialdried over anhydrous Na2SO4
  7. customthe solvents were removed under reduced pressure
  8. customThe residue thus obtained
  9. customwas purified by a filter column