Hydrochloric Acid → Zidovudine

温度

85 °C

The zidovudine guanidine salts from each of Compositions E and F were combined and thereafter added to a mixture of water (23 mL) and 32% hydrochloric acid (7.98 g) which had been heated to 85° C. The salts were completely dissolved in a few minutes and the pH of the mixture was 8.2. The pH was then adjusted to pH 1 by further addition of 32% hydrochloric acid the mixture was then cooled to ambient temperature and stirred for 16 hours. Thereafter, the mixture was further cooled to 5° C., stirred for 30 minutes, and filtered and washed with water to yield 15.74 g of substantially purified zidovudine--see Composition H in Table 1. The mother liquor from the production of Composition H was basified to pH 12.35 by addition of 50% sodium hydroxide to yield a precipitate which was filtered and washed with water to yield 2.18 g of zidovudine guanidine salt--see Composition I in Table 1--which was of sufficient purity to be recycled with other batches of zidovudine guanidine salts (i.e. combine with salts from Compositions E and F). The mother liquor was acidified to pH 1 and extracted several times with methyl isobutyl ketone and the combined extract was set aside.

1. dissolutionThe salts were completely dissolved in a few minutes
2. temperaturewas then cooled to ambient temperature
3. temperatureThereafter, the mixture was further cooled to 5° C.
4. stirringstirred for 30 minutes
5. filtrationfiltered
6. washwashed with water

ORDレコード

ord-6c99c719de2d4ab982c211c84305ffbd

出典データセット

uspto-grants-1996_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05519129