Hydrochloric Acid → HCID 3912385, compound

Participants

Reaction Steps

Commercially available 5-trifluoromethoxyisatin (5.66 g, 24.5 mmol) was added in small portions to an ethanol (75 mL) solution of potassium hydroxide (85%, 3.60 g, 54.5 mmol) under ice cooling. To the mixture, acetophenone (3.00 mL, 25.7 mmol) was further added, and then, the mixture was heated to reflux for 1 hour. After the reaction solution was concentrated, water was added to the residue, and then concentrated hydrochloric acid (4.47 mL, 53.6 mmol) was added thereto. The deposited crystal was collected by filtration, washed with water, and dried. The crude crystal was dissolved in a saturated aqueous solution of sodium bicarbonate and washed with diisopropyl ether, and then, concentrated hydrochloric acid was added until a crystal was deposited. The deposited crystal was collected by filtration, washed with water, and dried to obtain the title compound (7.06 g, 21.2 mmol) as an ocherous powder.

Provenance & Evidence