HRID600774
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
CONDITIONS
反应条件
- 温度
- 40 °C
PROCEDURE
实验过程
A solution of the product of Example 1H (150 mg, 0.375 mmol) in tetrahydrofuran (2.3 mL) was treated with 2N HCl (0.76 mL, 1.52 mmol), and the mixture was heated at 40° C. for 1 hour. After cooling to room temperature, the solution was brought to pH 8 with saturated NaHCO3 solution, and extracted with ethyl acetate. The organic extracts were washed with H2O, dried over Na2SO4, filtered and evaporated in vacuo to the title compound as a brown residue (140 mg, 100%). 1H NMR (DMSO-d6) δ 9.56 (s, 1H), 7.78 (m, 4H), 7.67 (d, 1H, J=7.8 Hz), 7.62 (s, 1H), 7.22 (t, 1H, J=7.8 Hz), 7.06 (d, 1H, J=7.4 Hz), 3.58 (s, 2H), 3.36 (m, 2H), 3.06 (t, 2H, J=6.8 Hz); MS (ESI+) m/z 373 (M+H)+.
WORKUP
后处理
- temperatureAfter cooling to room temperature
- extractionextracted with ethyl acetate
- washThe organic extracts were washed with H2O
- dry with materialdried over Na2SO4
- filtrationfiltered
- customevaporated in vacuo to the title compound as a brown residue (140 mg, 100%)