反应详情

To a solution of 4-[(2,3-difluoro-benzylidene)-amino]-1-methanesulfonyl-1H-pyrrole-2-carboxylic acid ethyl ester (500 mg, 1.40 mmol) in co-solvents of MeOH (10 mL) and DME (5 mL) was added TosMIC (410 mg, 2.10 mmol) and K2CO3 (390 mg, 2,82 mmol). The reaction mixture was heated under reflux for 2 hours and the solvents were removed by evaporation. The residue was treated with LiOH in THF/H2O at room temperature for 14 hours. After removal of the solvents by evaporation, the residue was acidified by 2N HCl solution. The crude product was then purified by HPLC to afford 50 mg desired product (12%). MS (ES−): m/e=288.0 (M−H); LC/Method A/2.45 min.

1. temperatureThe reaction mixture was heated
2. temperatureunder reflux for 2 hours
3. customthe solvents were removed by evaporation
4. additionThe residue was treated with LiOH in THF/H2O at room temperature for 14 hours
5. customAfter removal of the solvents
6. customby evaporation
7. customThe crude product was then purified by HPLC