Water → Chloroacetanilide

Participants

Reaction Steps

In accordance with the present invention there is provided a method for the preparation of a scintillographic agent which comprises dissolving 2,4-dimethylaniline in acetic acid at room temperature, mixing the resulting solution with chloracetyl chloride under vigorous mixing. The solution then is kept several hours at a temperature of 4° C. The reaction mixture is poured into water with ice. The sediment is crystallized from alcohol and from post-crystallizatic bases, diluted in water, a further quantity of sediment is regained which gives a total yield 80 to 82 %. The ω-chloracetanilide produced in this way is dissolved, together with the sodium salt of iminodiacetic acid, in aqueous ethanol wherein the proportion by volume of water to ethanol is 1:1.2. The mixture is warmed during several hours under a water circulation cooler. After the evaporation of solvent, the dry sediment is dissolved in water, the non-reacted component is separated, and the residual water solution is adjusted to the pH value about 2.5. The precipitated sediment is dissolved in absolute ethanol, non-reacted component is separated and, after the evaporation of solvent, the derivative of iminodiacetic acid is crystallized from water at pH about 2.5. The yield is 25 to 35 %. Further, the derivative of iminodiacetic acid, produced in this way, is dissolved in water with a possible addition of stannous chloride in hydrochloric acid and the pH value is adjusted to 4 to 6 depending on the supplied chelating radiometal. The solution is then passed through a sterile filter, freeze-dried and stored in sterile ampoules fixed in nitrogen or filled at a reduced pressure. At least half an hour prior to an intravenous administration the sterile solution of pertechnetate 99 m Tc or another radiometal is added to the derivative of iminodiacetic acid. The scintillographic agent according to the invention is durable up to 24 hours.

Provenance & Evidence