反应详情

4-Amino-3-iodo-N-methyl-benzenemethanesulfonamide (1.63 g, 0.005 mol), bis(trimethylsilyl)acetylene (1.28 g, 0.0075 mol) and tetrakistriphenylphosphine Pd(O) (0.578 g, 0.0005 mol) were dissolved in DME (50 mL) and followed by the addition of saturated aqueous Na2CO3 (5 mL). The mixture was heated at reflux for 48 h. The solvent was removed in vacuo. The residue was dissolved in EtOAc and extracted with brine. The organic layer was dried over Na2SO4, filtered and evaporated in vacuo. Silica gel chromatography (10-100% EtOAc gradient in hexane) of the residue afforded the product (4) (1.08 g, 76.8%).

1. temperatureThe mixture was heated
2. temperatureat reflux for 48 h
3. customThe solvent was removed in vacuo
4. dissolutionThe residue was dissolved in EtOAc
5. extractionextracted with brine
6. dry with materialThe organic layer was dried over Na2SO4
7. filtrationfiltered
8. customevaporated in vacuo