Hydrochloric Acid → HCID 22363603, compound

Participants

Reaction Steps

100 ml of 1N sodium hydroxide solution is added to a solution of 18.9 g of sodium borohydride in 100 ml of water. A solution of 163.6 g of 1-methylperhydroazepin-4-one HCl in 100 ml of water is added dropwise at an internal temperature of 0° to 5° C. The mixture is stirred for 2 hours at 0° to 5° C. and then for 2 hours at room temperature. The pH is adjusted to 2 to 3 by addition of semi-concentrated hydrochloric acid. The mixture is evaporated to dryness in vacuo, the residue is taken up in 600 ml of isopropanol, the inorganic salts are separated off at 60° to 75° C. and the product is crystallised in an ice bath. The product is filtered and dried to constant weight in vacuo at elevated temperature. 149 g (90%) of 1-methylperhydroazepin-4-ol HCl is obtained.

Provenance & Evidence