反应详情

To a solution of the compound (2.40 g) obtained in Step 2, 4-trifluoromethoxybenzylamine (1.21 g) and 1-hydroxybenzotriazole hydrate (1.21 g) in N,N-dimethylformamide (24 ml) was added, with stirring under ice-cooling, 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride (1.21 g). After stirring overnight at room temperature, and the reaction mixture was partitioned by adding ethyl acetate and water. The organic layer was washed successively with saturated aqueous sodium hydrogen carbonate solution, 10% aqueous citric acid solution and saturated brine, dried over anhydrous magnesium sulfate, filtrated, and concentrated under reduced pressure. The obtained crude crystals were suspended in a mixed solution of diisopropyl ether and n-hexane, collected by filtration and dried to give the title compound (2.20 g).

1. temperaturecooling
2. stirringAfter stirring overnight at room temperature
3. customthe reaction mixture was partitioned
4. additionby adding ethyl acetate and water
5. washThe organic layer was washed successively with saturated aqueous sodium hydrogen carbonate solution, 10% aqueous citric acid solution and saturated brine
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationfiltrated
8. concentrationconcentrated under reduced pressure
9. customThe obtained crude crystals
10. filtrationcollected by filtration
11. customdried