Lithium iodide → HCID 70136544, compound

Participants

Reaction Conditions

Reaction Steps

Lithium iodide (4.0 g, 29.7 mmol) was added to a solution of 6-[3-(2,4,6-trichlorobenzoyl)-6-methoxybenzyl]-2H-pyridazin-3-one (2.5 g, 5.9 mmol) [prepared by proceeding as described in Example 3, but replacing 2-fluorophenylacetic acid with 2-methoxyphenylacetic acid] in 2,4,6-collidine (250 ml) and the reaction mixture was heated to 165° C. After 3 h the reaction mixture was cooled to room temperature, and the product was extracted into ethyl acetate. The organic extract was washed with aqueous HCl (5%), NaHCO3 and brine, and dried over MgSO4. The organic solvent was removed in vacuo to give 2.25 g of crude product, which upon recrystallization from chloroform/hexanes gave pure 6-[3-(2,4,6-trichlorobenzoyl)-6-hydroxybenzyl]-2H-pyridazin-3-one (1.97 g) as a solid, mp 257.8° C.

Provenance & Evidence