反应详情

温度

70 °C

A solution of 6-[(2-chloro-α,α,α,6-tetrafluoro-p-tolyl) oxy]-α-methyl-1H-benzotriazole-1-acetaldehyde dimethyl acetal (20 g, 0.046 mole) in acetic acid is treated with 47 ml of 2.5N H2SO4, heated for 12 hours at 70° C., cooled and diluted with water and methylene chloride. The phases are separated and the aqueous phase is extracted with methylene chloride. The combined organic phases are dried (MgSO4), filtered through a pad of Al2O3, and concentrated in vacuo to afford the title compound as a solid, mp 107°-108° C., characterized by elemental and NMR analyses.

1. temperaturecooled
2. customThe phases are separated
3. extractionthe aqueous phase is extracted with methylene chloride
4. dry with materialThe combined organic phases are dried (MgSO4)
5. filtrationfiltered through a pad of Al2O3
6. concentrationconcentrated in vacuo