HRID710336
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
To a stirred solution of 4-bromo-N-(3-methoxyphenyl)benzenesulphonamide (0.5 g 1.46 mmol) and K2CO3 (0.5 g) in anhydrous DMF (7 ml) MeI (1 ml) was added and this was stirred at 50° C. for 0.5 h. The mixture was diluted to 50 ml with H2O and extracted in EtOAc (50 ml). The organic layer was washed with H2O, dried over MgSO4, filtered and the filtrate was passed through silica gel bead. The filtrate was evaporated to dryness to give the product (0.5 g; 96%), as a pale solid. 1H-NMR (CDCl3) 3.14 (5, 3H); 3.75 (s, 3H); 6.58 (broad d, 1H), 6.69 (t, 1H, J=2.20 Hz); 6.80 (dd, 1H, J=2.5, 8.34, Hz); 7.18 (tr, 1H, J=8.15 Hz); 7.40 (d, 2H, J=8.67 Hz); 7.58 (d, 2H, J=8.64 Hz).
WORKUP
后处理
- extractionextracted in EtOAc (50 ml)
- washThe organic layer was washed with H2O
- dry with materialdried over MgSO4
- filtrationfiltered
- customThe filtrate was evaporated to dryness
- customto give the product (0.5 g; 96%)