Hydrochloric Acid → HCID 86615025, compound

Participants

Reaction Steps

178 ml of hydrochloric acid (32%, excess) were added rapidly at 0° C. to a solution of 7-dimethylaminomethyl-8-(2-methyl-phenyl)-1,4-dioxa-spiro[4.5]decan-8-ol hydrochloride (73.5 g, 215 mmol) in tetrahydrofuran/water mixture, and stirring was then carried out for 16 hours at RT. The mixture was adjusted to pH 12 with 32% sodium hydroxide solution, and extraction was carried out with ether. After evaporation of the solvent in vacuo, the residue was taken up in diisopropyl ether and EE, and the corresponding salt was precipitated by addition of methanesulfonic acid (13 ml, 200 mmol). 64.3 g (84%) of the product were obtained in the form of a colorless solid.

Provenance & Evidence