反应详情

150 g of aluminum chloride were added over 30 minutes at 40° C under an argon atmosphere to a suspension of 107.8 g of 2-methyl-3-nitro-benzoyl chloride (Step A -- Example IV) in 450 ml of fluorobenzene and the mixture was held at this temperature for 41 hours. After icing, the mixture was added to 1 liter of ice water and 250 ml of concentrated hydrochloric acid and after stirring for 30 minutes, the mixture was extracted with methylene chloride. The extract was washed with water, then with N sodium hydroxide and then with water until the wash water was neutral. The solution was dried over magnesium sulfate, treated with activated carbon, filtered and evaporated to dryness under reduced pressure to obtain 115.7 g of 2-methyl-3-nitro-4'-fluorobenzophenone in the form of white crystals. For analysis, a sample of the product was crystallized from n-pentane and had a melting point of 64° C.

1. extractionthe mixture was extracted with methylene chloride
2. washThe extract was washed with water
3. dry with materialThe solution was dried over magnesium sulfate
4. additiontreated with activated carbon
5. filtrationfiltered
6. customevaporated to dryness under reduced pressure