A: Infrared Absorption 197K.

B: Dissolve about 100 mg in 50 mL of 1 N sodium hydroxide, and reflux for 15 minutes. Cool, and add 3 mL of the refluxed solution to 25 mL of saturated sodium bicarbonate solution. Add, with mixing, 4 mL of N,N-dimethyl-p-phenylenediamine dihydrochloride solution (1.5 in 10,000) and 2 mL of sodium hypochlorite solution (1.5 in 20,000): a violet-blue color is produced.

C: Dissolve about 50 mg in 20 mL of water, add 10 mL of a 1 in 50 solution of ammonium reineckate in methanol, and allow to stand for 30 minutes with occasional swirling: a pink reineckate of demecarium forms, and it melts between 131 and 136, with decomposition.

D: A solution of it responds to the tests for Bromide 191.

Control solution— Dissolve 100 mg of m-dimethylaminophenol in 10 mL of alcohol in a 1000-mL volumetric flask, dilute with water to volume, and mix. Pipet 1 mL of this solution into a 500-mL volumetric flask, dilute with water to volume, and mix.

Test solution— Transfer 100 mg of Demecarium Bromide to a 100-mL volumetric flask, add water to volume, and mix.

Procedure— Pipet 25 mL of the Test solution into a glass-stoppered, 50-mL centrifuge tube, and pipet 25 mL of the Control solution into a second, similar tube. To each tube add 3 mL of pH 7.0 phosphate buffer (see under Solutions in the section Reagents, Indicators, and Solutions), 1 mL of N,N-dimethyl-p-phenylenediamine dihydrochloride solution (1.5 in 10,000), 5 mL of isobutyl alcohol, and 1 mL of sodium hypochlorite solution (1.5 in 20,000). Insert the stoppers in the tubes, shake the mixtures for 5 minutes, and centrifuge: any blue color produced in the upper layer obtained from the Test solution is not more intense than that obtained from the Control solution.

(Official January 1, 2007)