HRID1748018
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
Platinum(IV) oxide (30 mg) was added to a solution of 9-{4-[3-(1,1-difluoroethyl)phenoxy]phenyl}-3,4-dihydropyrido[2,1-c][1,2,4]thiadiazine 2,2-dioxide (230 mg) in THF (dry) (20 mL) and MeOH (20 mL). The mixture was stirred at room temperature under hydrogen overnight. Activated carbon was added and the insoluble solid was removed by filtration through NH-silica gel/Celite pad (eluted with EtOAc) and the filtrate was concentrated in vacuo. The residue was purified by column chromatography (silica gel, eluted with MeOH in EtOAc) and concentrated. The residue was crystallized from EtOAc/hexane to give the title compound (79.4 mg) as colorless crystals.
WORKUP
后处理
- additionActivated carbon was added
- customthe insoluble solid was removed by filtration through NH-silica gel/Celite pad (eluted with EtOAc)
- concentrationthe filtrate was concentrated in vacuo
- customThe residue was purified by column chromatography (silica gel, eluted with MeOH in EtOAc)
- concentrationconcentrated
- customThe residue was crystallized from EtOAc/hexane