Hydrochloric Acid → HCID 59314174, compound

Participants

Reaction Conditions

Reaction Steps

A stirred solution of sodium hypochlorite (5.25% Aqueous, 204 mL, 143 mmol) and 2N aqueous KOH (22 mL, 44 mmol) are heated to 50° C. and 1-(4-difluoromethoxy-2-methyl-phenyl)-ethanone (A4) (5.8 g, 29 mmol) is added. After maintaining the temperature at 50-70° C. for 3 h and keeping at RT overnight, the reaction is reheated to 50° C. and sodium metabisulfite (4.5 g) is added in 3 portions. The reaction is then acidified with 12N HCl and stirred well. The precipitated white solid is filtered off, rinsed with a little water and air dried to afford 4-difluoromethoxy-2-methyl-benzoic acid (242) (5.4 g, 92%). The product is recrystallized from 1:1 mixture of ACN and water. mp: 117-119° C. Elemental Analysis: Actual C (53.23), H (3.88), F (18.66) Theoretical C (53.47), H (3.99), F (18.80).

Provenance & Evidence