Hydrochloric Acid → HCID 13069856, compound

Participants

Reaction Steps

To 7.0 g (0.07697 mole) of the sodium salt of 1H-1,2,4-triazole, generated from 5.3 g; (0.07697 mole) of 1H-1,2,4-triazole and 3.1 g (0.759 mole) of NaOH, in 50 ml of DMSO, is added 30.0 g (0.0767 mole) of 2-cyano-2-(2,4-dichlorophenyl) decyl bromide (prepared by the usual route); and the reaction is stirred at 130° for 20 hours. The mixture is then cooled and mixed with 200 ml of water. The organic material which separates is extracted 2×100 ml of ether, and the extract is washed 2×50 ml of water, dried over anhydrous magnesium sulfate and concentrated to give 24.0 g (82.5%) of the crude product. This material is dissolved in ether, and it is treated with hydrogen chloride gas until it is acidic to litmus. The solid which precipitates is separated by filtration to give 9.0 g (28.2%) of the hydrochloric salt, mp 125°-31°. To 6.7 g (0.0161 mole) of the hydrochloride salt in 200 ml of water is stirred. The organic soluble material is extracted 2×200 ml of ether, and the extract is washed 2×50 ml of water, dried over anhydrous magnesium sulfate, and concentrated to give 4.9 g (80.2%) of the oil product.

Provenance & Evidence