Ethanolamine hydrochloride (3.3g) is dissolved in 6.6mlDMSOby gentle heating to ~70°C, subsequently 10% (v/v) of molecular sieves (0.4nm) are added. The solution is allowed to cool to RT. Dissolved air is removed by degassing in adesiccatorataspiratorvacuum for 30min. The cantilevers ar...
Suitable physiologically acceptable salts of the compounds of general formula (I) include acid addition salts derived from inorganic and organic acids, such as hydrochlorides, hydrobromides, sulphates, phosphates, maleates, tartrates, citrates, benzoates, 4-methoxybenzoates, 2 or 4-hydroxybenzoates,...
This crude hydrochloride was dissolved in ethanol (283 ml) and the stirred solution was treated with a solution of NaOH (3.53 g) in H2 O (3.53 ml) keeping the temperature below 20°. The solution was cooled to below 10°, and a solution of NaBH4 (9.15 g) and NaOH (1.26 g) in H2...
The solutions were mixed well and 0.3 M sodium hydroxide (0.3 mL) and 0.5 M hydroxylamine hydrochloride (0.1 mL) were added. The final volume adjusted to 2 mL with acetic acid. The UV spectra of the solutions were measured against a blank prepared using the same method, ...
(B) Analogously to Example 21A. from 697 mg of methyl p-[(R)-2-[[(S)-2-(6-chloro-2-pyridyl)-2-hydroxyethyl]amino]propyl]benzoate there were obtained 420 mg of amorphous p-[(R)-2-[[(S)-2-(6-chloro-2-pyridyl)-2-hydroxyethyl]amino]propyl]benzoic acid hydrochloride, [α]D20=+...
pH at 9-10. After cooling to ambient temperature the pH of the solution is adjusted to 2.5 with aqueous HCl. The resulting precipitate is collected by filtration, washed with acetone, and dried in vacuo to afford the mono-hydrochloride salt of 1,4,7-tricarboxymethyl-1,4,7-triazacyclo...
(B) Analogously to Example 21A, from 697 mg of methyl p-[(R)-2-[[(S)-2-(6-chloro-2-pyridyl)-2-hydroxyethyl]amino]propyl]benzoate there were obtained 420 mg of amorphous p-[(R)-2-[[(S)-2-(6-chloro-2-pyridyl)-2-hydroxyethyl]amino]propyl]benzoic acid hydrochloride, [α]D20=+...