反应详情

To a suspension of 5-amino-4-carboxy-1-(2,2-diethoxyethyl)pyrazole (4 g) in xylene (15.6 ml) was added dropwise 3.4M solution of sodium bis(2-methoxyethoxy)-aluminum hydride in toluene (15.6 ml) at room temperature in an atmosphere of nitrogen. Then the mixture was refluxed for 6 hours, and poured into a mixture of dichloromethane and water. The precipitate was filtered off, and the organic layer was separated and dried over magnesium sulfate. The organic solvent was evaporated in vacuo to give 5-amino-4-methyl-1-[(E)-2-ethoxyvinyl]-pyrazole (598 mg). IR (Nujol) : 3440, 3280, 3150, 1665, 1625, 1585, 1520 cm-1

1. temperatureThen the mixture was refluxed for 6 hours
2. filtrationThe precipitate was filtered off
3. customthe organic layer was separated
4. dry with materialdried over magnesium sulfate
5. customThe organic solvent was evaporated in vacuo