Acetic Acid → HCID 14324460, compound

Participants

Reaction Steps

After mixing 279 g of 5-methyl-2-(4-ethoxycarbonyl-2-nitrophenyl)isoxazolin-3-one prepared in the above step, 700 ml of acetic acid, 129 g of paraformaldehyde, 156 g of zinc chloride, and 20 ml of sulfuric acid, the reaction system was saturated with hydrogen chloride gas at room temperature and the reaction was performed for 8 hours in a steam bath while further blowing hydrogen chloride gas into the system. Thereafter, 200 ml of water was added to the system and the reaction was further performed for 2 hours. After the reaction was over, the reaction mixture was cooled and then 2 liters of water was added thereto. Crystals thus deposited were recovered by filtration, washed with water, and dried to provide 199 g of the desired product with a yield of 66.7%. The melting point thereof was 190° C. to 191° C. (decompd.).

Provenance & Evidence