反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
1-(3-(methylamino)-1-trityl-1H-pyrazolo[4,3-c]pyridin-6-yl)-3-(phenyl(tetrahydrofuran-2-yl)methyl)urea (320 mg, 0.526 mmol) was taken up in TFA (3.0 ml). Triethylsilane (0.126 ml, 0.789 mmol) was added and the reaction was allowed to stir at rt for 30 mins. The reaction mixture was concentrated in vacuo. Saturated NaHCO3 was slowly added. The products were then washed with EtOAc (3×). The combined organic layers were then washed with brine, dried over MgSO4, filtered through celite, then concentrated in vacuo. The oil was taken up in 2 ml of DCM and loaded directly onto silica gel. Purification by MPLC 0-15% EtOAc/MeOH gave 1-(3-(methylamino)-1H-pyrazolo[4,3-c]pyridin-6-yl)-3-(phenyl(tetrahydrofuran-2-yl)methyl)urea. MS ESI calc'd. for C19H23N6O2 [M+H]+ 367. found 367.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated in vacuo
- additionSaturated NaHCO3 was slowly added
- washThe products were then washed with EtOAc (3×)
- washThe combined organic layers were then washed with brine
- dry with materialdried over MgSO4
- filtrationfiltered through celite
- concentrationconcentrated in vacuo
- customPurification by MPLC 0-15% EtOAc/MeOH