HRID44851
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
Three mL of TFA was added to a solution of (R)-tert-butyl 4-(8-cyclopentyl-7-ethyl-5-methyl-6-oxo-5,6,7,8-tetrahydropteridin-2-yl)pyridin-3-ylcarbamate (Example 92, 760 mg) in 3 mL of DCM. The mixture was stirred for 4 h at rt, and the solvent was removed under reduced pressure. Aqueous Na2CO3 was added and extracted with EtOAc. The organic layer was dried with Na2SO4, concentrated and the residue was purified by silica column to give the title compound. LCMS (0.05% TFA): 353.0 m/z (M+H)+; 1H-NMR (CDCl3, 500 MHz): δ: 8.17 (s, 1H), 8.08 (d, 1H, J=5 Hz), 7.99 (d, 1H, J=5 Hz), 7.94 (s, 1H), 6.23 (s, 2H), 4.48 (m, 1H), 4.32 (m, 1H), 3.39 (s, 3H), 2.0-1.69 (m, 10H), 0.88 (t, 3H, J=7.5 Hz).
WORKUP
后处理
- customthe solvent was removed under reduced pressure
- additionAqueous Na2CO3 was added
- extractionextracted with EtOAc
- dry with materialThe organic layer was dried with Na2SO4
- concentrationconcentrated
- customthe residue was purified by silica column