反应详情

温度

2 °C

To a 100 ml volume four-necked flask, methanol (22.91 g) and hydrazine hydrate (1.93 g) were added at room temperature, and cooled. Ethyl 2-(2,6-diethyl-4-methylphenyl)-2-oxoacetate (9-a) (5.01 g) diluted with methanol (10.02 g) was added dropwise at 1° C. over 5 minutes. The resulting mixture was stirred at 2° C. for 4 hours, then the mixture was filtered. The resulting filtrate was concentrated, added tert-butyl methyl ether (41 g), and washed with brine (14 g). The resulting organic layer was dried over sodium sulfate, and concentrated under reduced pressure. The residue was subjected to column chromatography (silica gel: 40 g, hexane:ethyl acetate=1:1) to gave 1.88 g of 2-(2,6-diethyl-4-methylphenyl)-2-oxoacetohydrazide ((12-1)-(11)-39).

1. temperaturecooled
2. additionwas added dropwise at 1° C. over 5 minutes
3. filtrationthe mixture was filtered
4. concentrationThe resulting filtrate was concentrated
5. additionadded tert-butyl methyl ether (41 g)
6. washwashed with brine (14 g)
7. dry with materialThe resulting organic layer was dried over sodium sulfate
8. concentrationconcentrated under reduced pressure