Synthetic Route of 1116-77-4, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 1116-77-4 as follows.
Example 3Reaction of 4-(1,2,4-triazol-1-yl-methyl)phenyl-hydrazine (IV) with 4-N,N-dimethylamino-butyraldehyde diethyl acetal (X) (Fischer indole synthesis)To the aqueous hydrazine (IV) solution obtained in example 2, conc. sulfuric acid (4.371) was added and the temperature of the reaction mixture was maintained for 2 hours at 65-70 C. After cooling to 20-25 C., 4-N,N-dimethylamino-butyraldehyde diethyl acetal (X) (3.15 kg) was added. The reaction was heated to 70 C. and maintained for 3-4 hours. After completion of the reaction, the reaction mixture was allowed to cool to 15-20 C. To this mixture, 25% aq. ammonia (7.251) was added to adjust the pH to 8.5-9. The solution was extracted with ethyl acetate (4×12.251). A solution of succinic acid (2.45 kg) in water (301) was added to the ethyl acetate extract. The mixture was stirred for 15 minutes. The aqueous layer was separated and washed with ethyl acetate (2×51). The aqueous layer was basified with 20% aq. NaOH to adjust the pH to 8.5-9. The solution was extracted with ethyl acetate (4 x 51). The combined ethyl acetate extracts were concentrated to give rizatriptan free base (VII) as oil (2.8 kg, 75.5% from 4-(1,2,4-triazol-1-yl-methyl)phenylamine (II)). Purity =99.7-99.9% (as measured by HPLC).
According to the analysis of related databases, 1116-77-4, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Gore, Vinayak G.; Kulkarni, Vikas S.; Wavhal, Sneha R.; US2010/256208; (2010); A1;,
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