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
A mixture of 2,2,2-trifluoro-N-(3-oxo-1-{4-[9-phenyl-3-(2-pyrimidinyl)[1,2,4]triazolo[3,4-f]-1,6-naphthyridin-8-yl]phenyl}cyclobutyl)acetamide (4-2) (25 mg, 0.043 mmol), trimethylsilyl cyanide (0.012 mL, 0.086 mmol), and zinc iodide (1.4 mg, 0.0043 mmol) in CH2Cl2 (1.0 mL) was stirred at room temperature for 1 hour. To the mixture was added water, extracted with CHCl3, washed with brine, dried (MgSO4), filtered, and the solvent was removed under reduced pressure. The residue was purified by preparative TLC, eluting with 10% MeOH in CHCl3 to give N-(3-cyano-3-hydroxy-1-{4-[9-phenyl-3-(2-pyrimidinyl)[1,2,4]triazolo[3,4-f]-1,6-naphthyridin-8-yl]phenyl}cyclobutyl)-2,2,2-trifluoroacetamide (4-10) as a yellow solid. MS (M+H)+: observed=607, calculated=607.
WORKUP
后处理
- extractionextracted with CHCl3
- washwashed with brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- customthe solvent was removed under reduced pressure
- customThe residue was purified by preparative TLC
- washeluting with 10% MeOH in CHCl3