Hydrochloric Acid → HCID 42600053, compound

Participants

Reaction Conditions

Reaction Steps

Ethyl acetate (10 mL) was added to a mixture of compound of example 38 (150 mg, 0.29 mol) and KBr in water (0.5 M, 0.24 mL), followed by addition of TEMPO (3.12 mg, 0.02 mmol). A solution of 12% NaClO in water (27 mg, 0.36 mmol) was added dropwise to the mixture over 30 minutes at 5° C. at pH of 8.0-10.0. Stirring was continued for 30 minutes at room temperature (25° C.). Then, the pH was adjusted to 5.0 by addition of 35% hydrochloric acid, followed by addition of 25% NaClO2 in water (32.8 mg, 0.36 mmol) over 30 minutes maintaining the temperature of 27-33° C. Stirring was continued for 3 hours at room temperature (25° C.). The product was extracted with ethyl acetate (3×50 mL), washed with brine, followed by concentration to obtain the title compound.

Provenance & Evidence