Hydrochloric Acid → HCID 178515569, compound

Participants

Reaction Steps

200 ml of water and 300 ml of ethanol were added to 40 g of sodium hydroxide to dissolve the sodium hydroxide. 69.5 g of hydroxylamine hydrochloride was added thereto, and the pH of the solution was adjusted to 10.0 by adding a 2N sodium hydrochloride ethanol/water (3:2) solution mixture. Under cooling with ice, 192 g of ethyl benzoylacetate and a 2N sodium hydroxide in ethanol/water (3:2) solution mixture were added dropwise simultaneously to the reaction solution so that the pH of the reaction solution was 10±0.3. After completion of the addition and stirring for 3 hours at room temperature, the reaction mixture was poured to a mixture of 500 g of concentrated hydrochloric acid and 500 g of ice, then 2.5 liters of ethanol was added to the reaction mixture and after the reaction mixture was heated for 3 hours under reflux, 2 liters of water was added thereto followed by cooling. The precipitated crystals were filtered, washed with water and dried.

Provenance & Evidence