反应详情

To a 500 ml volume four-necked flask, 1-[(2,6-diethyl-4-methylphenyl)-2-oxoacetyl]-1-methyl-2-(1-methylethylidene)hydrazine (18-a) (21.41 g) and tetrahydrofuran (150 ml) were added under a nitrogen atmosphere at room temperature. To the mixture, 10% by weight of hydrochloric acid (29.23 g) was added dropwise over 5 minutes, and stirred at room temperature for 1 hour. Then, the reaction mixture was concentrated under reduced pressure. To the residue was added water (60 ml), and extracted with tert-butyl methyl ether. The organic layer was concentrated under reduced pressure, and added hexane (50 ml). The precipitated crystal was collected by filtration and dried to give 12.70 g of 1-[2-(2,6-diethyl-4-methylphenyl)-2-oxoacetyl]-1-methylhydrazine ((12-2)-(11)-39).

1. concentrationThen, the reaction mixture was concentrated under reduced pressure
2. additionTo the residue was added water (60 ml)
3. extractionextracted with tert-butyl methyl ether
4. concentrationThe organic layer was concentrated under reduced pressure
5. additionadded hexane (50 ml)
6. filtrationThe precipitated crystal was collected by filtration
7. customdried