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-(1,5-dimethyl-2,4-dioxo-6-(3-(trifluoromethoxy)phenyl)-1H-pyrrolo[3,2-d]pyrimidin-3(2H,4H,5H)-yl)propyl acetate (30 mg, 0.068 mmol) in THF (5 mL) and water (5 mL) was added LiOH.H2O (5.73 mg, 0.136 mmol). The reaction was stirred at RT for 30 min then diluted with DCM (5 mL) and water (5 mL). The organic layer was dried over Na2SO4 and concentrated to a residue which was purified by Prep HPLC to give 3-(3-hydroxypropyl)-1,5-dimethyl-6-(3-(trifluoromethoxy)phenyl)-1H-pyrrolo[3,2-d]pyrimidine-2,4(3H,5H)-dione (10 mg, 36.9% yield) as a white solid. 1H NMR (CDCl3) δ: 7.54 (t, J=7.9 Hz, 1H), 7.38 (d, J=7.8 Hz, 1H), 7.32 (d, J=11.0 Hz, 2H), 6.03 (s, 1H), 4.29-4.17 (m, 2H), 3.98 (s, 3H), 3.72 (s, 1H), 3.54 (t, J=5.1 Hz, 2H), 3.50 (s, 3H), 1.99-1.84 (m, 2H). LCMS: MH+ 398 and TR=2.507 min.
WORKUP
后处理
- dry with materialThe organic layer was dried over Na2SO4
- concentrationconcentrated to a residue which
- customwas purified by Prep HPLC