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 solution of 2,4,6-trimethoxystyryl-3-(3,5-dinitrobenzamido)-4-methoxy-benzylsulfone (example 5) (1.3 mmol) in acetone water (10:5) was heated to 50° C. After 30 min, sodiumhydrosulfite (Na2S2O4) (26.3 mmol) was added slowly, and the mixture was heated at reflux (50° C., 1 h.), cooled to room temperature and water was added. The product was rinsed with NaHCO3, and then isolated by extraction with ethyl acetate. The organic layer was dried over-anhydrous Na2SO4. The solvent was removed under reduced pressure and the crude product was recrystallized from 2-propanol to yield pure (E)-2,4,6-trimethoxystyryl-3-(3,5,diaminobenzamido)-4-methoxy-benzylsulfone. m.p. 208-210° C. NMR (DMSO-d6) δ 3.76 (s, 3H), 3.80 (s, 6H), 3.82 (s, 3H), 4.4 (s, 2H), 5.9 (s, 1H), 6.2 (s, 2H), 7.05-8.26 (m, aromatic), 8.85 (s, 1H).
WORKUP
后处理
- temperaturethe mixture was heated
- temperaturecooled to room temperature
- washThe product was rinsed with NaHCO3
- customisolated by extraction with ethyl acetate
- customThe solvent was removed under reduced pressure
- customthe crude product was recrystallized from 2-propanol