HRID1746026
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
- 50 °C
PROCEDURE
实验过程
A well-stirred solution of 2′,3′-Dinitro-3,4,4′,5-tetramethoxy-(Z)-stilbene (0.422 g, 1.08 mmol) in a mixture of acetone-water (2:1) was heated to 50° C. Then sodium thiosulfate (1.88 g, 10.81 mmol, 10.0 equiv) was added and the reaction mixture was heated to reflux for 6 hours. The reaction was cooled to room temperature and water was added. The organic layer was separated and the aqueous layer was extracted with ethyl acetate (4×25 mL). The combined organic layer were washed with brine, dried over Na2SO4 and concentrated in vacuo. The mixture was then subjected to preparative TLC to give the 2′,3′-Diamino-3,4,4′,5-tetramethoxy-(Z)-stilbene.
WORKUP
后处理
- temperaturethe reaction mixture was heated
- temperatureto reflux for 6 hours
- temperatureThe reaction was cooled to room temperature
- customThe organic layer was separated
- extractionthe aqueous layer was extracted with ethyl acetate (4×25 mL)
- washThe combined organic layer were washed with brine
- dry with materialdried over Na2SO4
- concentrationconcentrated in vacuo