反应详情

A solution of 5-(2,2,2-trichloroethoxycarbonyl)amino-3-t-butyl-1-p-tolylpyrazole (26 mmol), 1-amino4-(2-pyridin-4-yl-ethenyl)naphthalene (26 mmol), diisopropylethylamine (3.2 g, 25 mmol) and DMSO (75 mL) is heated to 55-90° C. and held for 2-8 h. To this solution, ethyl acetate (100 mL) is added. The organic layer is washed with brine (4×50 mL), and dried over MgSO4. The solvent is removed under reduced pressure, and residue is crystallized from a suitable solvent such as acetonitrile (50 mL) at 020 C. The product is collected by filtration and recrystallized from a suitable solvent such as isopropanol and dried in vacuum to constant weight.

1. washThe organic layer is washed with brine (4×50 mL)
2. dry with materialdried over MgSO4
3. customThe solvent is removed under reduced pressure, and residue
4. customis crystallized from a suitable solvent such as acetonitrile (50 mL) at 020 C
5. filtrationThe product is collected by filtration
6. customrecrystallized from a suitable solvent such as isopropanol
7. customdried in vacuum to constant weight