Hydrochloric Acid → HCID 14519825, compound

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Reaction Steps

The oil obtained in stage c (14 g) is dissolved in 50 ml of water and 8.1 g of concentrated hydrochloric acid and the solution is cooled to -5° C. A solution of 6.6 g of potassium cyanide in 20 ml of water is then added dropwise. After addition of 15 ml of ethanol, a 39% strength formalin solution (8.2 g) is added dropwise and the pH of the mixture is brought to 7. The mixture is stirred at room temperature for 2 hours and brought to pH 1.5 with concentrated hydrochloric acid, and a solution of 5.6 g of sodium nitrite in 25 ml of water is added dropwise, while cooling with ice. The mixture is subsequently stirred at room temperature overnight and then extracted with diethyl ether, and the extract is dried and concentrated. The oil which remains is dissolved in 50 ml of concentrated methanolic hydrochloric acid and the solution is diluted with 50 ml of ethyl acetate. The precipitate which has separated out is filtered off with suction and discarded. After 2 hours, the filtrate is concentrated, the residue is stirred with ethyl acetate and the solid is filtered off with suction and recrystallized from ethanol/diethyl ether (1:2). Yield: 5.9 g melting point=161°-163° C. (decomp.)

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