Sulfuric Acid → 4-Chloromethyl-5-phenyl-2-(4-carboxy-2-nitrophenyl)-4-isoxazolin-3-one

Participants

Reaction Steps

After adding 300 ml of concentrated sulfuric acid to a mixture of 270 g (0.67) of 4-chloromethyl-5-phenyl-2-(4-ethoxycarbonyl-2-nitrophenyl)-4-isoxazolin-3-one (Compound (33)) and 2.5 liters of 1,4-dioxane, the resultant mixture was refluxed for 8 hours. Thereafter, the reaction mixture obtained was cooled and poured into water. Crystals thus deposited were recovered by filtration, washed with water, and dried to provide 210.2 g of the aforesaid compound with a yield of 83.7%. The melting point thereof was 186° C. to 189° C.

Provenance & Evidence