反应详情

3-methyl-2-pyridinamine (1.3 g, 12 mmol) was dissolved in dry pyridine (20 ml) and ethyl 2- acetyloxy-5-[(4-chlorosulfonylphenyl)ethynyl]-benzoate (4.1 g, 10 mmol) was added. The solution was kept at ambient temperature for 18 h. The solvent was evaporated and the residue dissolved in a small amount of tetrahydrofuran. The solution was added to a refluxing solution of potassium hydroxide (6 g) in water (100 ml) and ethanol (50 ml). After 15 min the solution was acidified with formic acid to produce a precipitate. The solid was collected by filtration, washed with water and dried. Yield 1.2 g, 29%.

1. customThe solvent was evaporated
2. dissolutionthe residue dissolved in a small amount of tetrahydrofuran
3. additionThe solution was added to a refluxing solution of potassium hydroxide (6 g) in water (100 ml) and ethanol (50 ml)
4. waitAfter 15 min the solution was acidified with formic acid
5. customto produce a precipitate
6. filtrationThe solid was collected by filtration
7. washwashed with water
8. customdried