反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe contents were heated to reflux
- customquenched with 1N HCl (5 mL)
- additionThe reaction mixture was further diluted with EtOAc (25 mL)
- customthe organic layer was separated
- washThe organic layer was washed with brine (1×20 mL)
- dry with materialdried over anhydrous Na2SO4
- customthe solvents were removed under reduced pressure
- customThe residue thus obtained
- customwas purified by a filter column