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 compound 80c (43.4 mg, 0.0860 mmol) in THF (2 mL) and EtOH (2 mL) was added 1N NaOH (1.00 mL, 1.00 mmol) and the resulting mixture was stirred at rt for 3.5 h. The solvents were removed under reduced pressure. The residue obtained was treated with EtOAc (20 mL) and water (20 mL). The resulting mixture was neutralized with 2N hydrochloric acid. The EtOAc layer was separated and the aqueous layer was extracted with EtOAc (20 mL). The combined organic layers were dried over Na2SO4, filtered, and concentrated under reduced pressure to yield the title compound 9. 1H-NMR (DMSO-d6) δ (ppm): 13.24 (br s, 1H), 8.49 (m, 3H), 8.05 (m, 3H), 7.86 (t, J=7.6 Hz, 1H), 7.79 (d, J=8.4 Hz, 1H), 7.74-7.61 (m, 2H), 5.08 (s, 2H), 4.22 (m, 4H), 3.82 (m, 4H). Mass Spectrum (LCMS, ESI pos.) Calcd. For C26H21N2O3 (M+H) 480.2. Found 480.4.
WORKUP
后处理
- customThe solvents were removed under reduced pressure
- customThe residue obtained
- customThe EtOAc layer was separated
- extractionthe aqueous layer was extracted with EtOAc (20 mL)
- dry with materialThe combined organic layers were dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure