HRID1518287
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
Compound 31C (3.1 g, 10.68 mmol) was dissolved in EtOH (20 mL). To this solution was added hydrazine hydrate (0.622 mL, 12.81 mmol). The reaction was heated under reflux for 2 hours. The solvent was removed, and the residue was taken up into EtOAc. It was then washed with water, brine, dried over MgSO4, and concentrated under reduced pressure to provide 2.72 g of the desired product: 1H NMR (DMSO-d6): δ 12.64 and 11.99 (s, 1H), 7.71-7.74 (m, 2H), 7.32-7.48 (m, 5H), 7.09-7.10 (br, 2H), 6.38 (s, 2H), 5.15 (s, 2H). MS (DCI(+)): m/z 291 (M+H).
WORKUP
后处理
- temperatureThe reaction was heated
- temperatureunder reflux for 2 hours
- customThe solvent was removed
- washIt was then washed with water, brine
- dry with materialdried over MgSO4
- concentrationconcentrated under reduced pressure