反应详情

A stirred solution of 2,6-dimethyl-3-nitrobenzene-1-methanol (51.3 g, 0.283 mole) and 25 ml of pyridine in 350 ml of toluene was warmed to 70°. During a ten minute period, acetyl chloride (22.2 g, 0.283 mole) was added to the reaction mixture. The reaction mixture was heated at 85° for 21/2 hours, then poured over 300 g of ice, and 100 ml of a 4N hydrochloric acid solution was added thereto. The organic phase was separated and washed with 100 ml of aqueous 2N hydrochloric acid, dried over anhydrous magnesium sulfate, and filtered. The solvent was removed from the filtrate under reduced pressure to give (2,6-dimethyl-3-nitrophenyl)methyl acetate (47.5 g) as an oil.

1. temperatureThe reaction mixture was heated at 85° for 21/2 hours
2. additionwas added
3. customThe organic phase was separated
4. washwashed with 100 ml of aqueous 2N hydrochloric acid
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationfiltered
7. customThe solvent was removed from the filtrate under reduced pressure