Ammonia → HCID 15383363, compound

Participants

Reaction Steps

1.35 g (4.9 mmol) of α-azidomethyl-2-chloro-5-sulphamoylbenzenemethanol, 90 ml of anhydrous pyridine and 9.67 g (29.0 mmol) of triphenylphosphine on a carrier are introduced into a 250-ml round-bottomed flask. The mixture is stirred at room temperature for 9 hours, 100 ml of 28% aqueous ammonia are then added, and the suspension is stirred for 16 hours and filtered. The filtrate is concentrated and the residue is recrystallized in methanol. 0.523 g of α-aminomethyl-2-chloro-5-sulphamoylbenzenemethanol is obtained. 1 equivalent of methanesulphonic acid in 2M solution in methanol is added. After recrystallization in methanol and diethyl ether and drying in a desiccator under vacuum over phosphorus pentoxide, 0.439 g of α-aminomethyl-2-chloro-5-sulphamoylbenzenemethanol methanesulphonate is obtained.

Provenance & Evidence