反应详情

To a solution of methyl 4-amino-3-fluoro-2-((2-fluorophenyl)amino)-5-((4-methoxybenzyl)thio)benzoate (9.79 g, 22.7 mmol) in anisole (12 mL) was added CF3COOH (20 mL). After stirring at ambient temperature for 23 h, the solvent was removed in vacuo. To the residue was added water (30 mL). The mixture was neutralized with 25% aqueous ammonia and extracted with ethyl acetate (100 mL×3). The combined organic layer was washed with water (100 mL×3) and brine (100 mL) sequentially, dried over Na2SO4, filtered and concentrated to give the desired product (white solid, 5.28 g, 75% yield). The product was used directly in the next step without further purification.

1. customthe solvent was removed in vacuo
2. additionTo the residue was added water (30 mL)
3. extractionextracted with ethyl acetate (100 mL×3)
4. washThe combined organic layer was washed with water (100 mL×3) and brine (100 mL) sequentially
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated