Packaging and storage
Preserve in well-closed, light-resistant containers.
Identification
B:
Dissolve about 500 mg of ammonium molybdate in 10 mL of sulfuric acid, and add to this solution about 2 mg of Hydroxyamphetamine Hydrobromide: an intense blue color is produced (distinction from similar amino compounds such as amphetamine and methamphetamine, which, lacking a phenolic hydroxyl, do not undergo this reaction).
C:
Dissolve about 200 mg in 2 mL of water, and add a solution of 500 mg of potassium carbonate in 2 mL of water. Extract with two 10-mL portions of ether, allow the clear ether solution to evaporate to dryness, and dry at about 80
: the hydroxyamphetamine so obtained melts between 124
and 127
(see
Class I under
Melting Range or Temperature 741).
D:
To a solution of about 10 mg of it in 10 mL of water add 1 mL of 2 N nitric acid, then add
silver nitrate TS: a pale yellow precipitate is formed, and it is slightly soluble in 6 N ammonium hydroxide.
Bromide content
Accurately weigh about 400 mg, and dissolve in 50 mL of water. Add 50 mL of methanol and 10 mL of glacial acetic acid, then add
eosin Y TS, and titrate with 0.1 N silver nitrate VS. Each mL of 0.1 N silver nitrate is equivalent to 7.990 mg of Br: the content of Br, calculated on the dried basis, is between 33.6% and 35.2%.
Ordinary impurities 466
Test solution:
methanol.
Standard solution:
methanol.
Eluant:
a mixture of toluene, methanol, and ammonium hydroxide (10:4:0.25).
Visualization:
1.
Assay
Dissolve about 400 mg of Hydroxyamphetamine Hydrobromide, accurately weighed, in a mixture of 10 mL of glacial acetic acid and 10 mL of
mercuric acetate TS, warming slightly, if necessary, to effect solution. Add
crystal violet TS, and titrate with 0.1 N perchloric acid VS. Perform a blank determination, and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 23.21 mg of C
9H
13NO·HBr.