反应详情

A mixture of N-tert-butyl-4-[(3-fluoro-4-methoxybenzylidene)amino]benzenesulfonamide (41.5 g, 114 mmol, obtained in example 2), tosylmethylisocyanide (33.22 g, 171 mmol), K2CO3 (31.1 g, 228 mmol), DME (340 mL) and MeOH (778 mL) is heated at reflux for 3 h. The solvent is removed and the residue is taken up in a CHCl3/H2O mixture and the layers are separated. The aqueous phase is extracted with CHCl3 and the combined organic extracts are dried over MgSO4 and concentrated. A crude product is obtained, which is washed with Et2O several times to give 41.40 g of a creamy solid that is directly used in the next reaction (yield: 90%).

1. temperatureis heated
2. temperatureat reflux for 3 h
3. customThe solvent is removed
4. customthe layers are separated
5. extractionThe aqueous phase is extracted with CHCl3
6. dry with materialthe combined organic extracts are dried over MgSO4
7. concentrationconcentrated
8. customA crude product is obtained
9. washwhich is washed with Et2O several times