Some common heterocyclic compound, 1116-77-4, name is 4,4-Diethoxy-N,N-dimethyl-1-butanamine, molecular formula is C10H23NO2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Formula: C10H23NO2
Example 3: Reaction of 4-(1.2.4-triazol-l-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, cone, sulfuric acid (4.371) was added and the temperature of the reaction mixture was maintained for 2 hours at 65- 700C. After cooling to 20-250C, 4-N,N-dimethylamino-butyraldehyde diethyl acetal (X) (3.15kg) was added. The reaction was heated to 700C and maintained for 3-4 hours. After completion of the reaction, the reaction mixture was allowed to cool to 15-200C. 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 x 12.251). A solution of succinic acid (2.45kg) 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 x 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 (2.8kg, 75.5% from 4-(l,2,4-triazol-l-yl- methyl)phenylamine (IT)). Purity = 99.7-99.9% (as measured by HPLC).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1116-77-4, its application will become more common.