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-(4-nitrobenzamido)-4-methoxybenzyl-sulfone (example 10) (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 give pure (E)-2,4,6-Trimethoxystyryl-3-(4-aminobenzamido)-4-methoxy-benzylsulfone. m.p. 137-140° C. NMR (DMSO-d6) δ 3.82 (s, 3H), 3.83 (s, 6H), 3.86 (s, 3H), 4.22 (s, 2H), 6.14 (s, 2H), 6.80-8.16 (m, aromatic), 8.60 (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
- dry with materialThe organic layer was dried over anhydrous Na2SO4
- customThe solvent was removed under reduced pressure
- customthe crude product was recrystallized from 2-propanol