Pyrazine drug as well as preparation method thereof, composition and application in gastrointestinal patient nursing
A composition, drug technology, applied in the field of clinical care, which can solve the problem of less choice for doctors and patients
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Embodiment 1
[0051] Step a): 1,4-dicyano-2,3-diamino-2-butene of formula (6) obtains a compound of formula (5) through acylation reaction and condensation reaction of amine aldehyde into a ring: at 0 Under the condition of ℃, slowly add the concentrated sulfuric acid to the water, add 1,4-dicyano-2,3-diamino-2-butene after the dropwise addition, then slowly raise the temperature, continue to slowly add the glyoxylic acid Aqueous solution, continue to heat up to reflux reaction, then slowly cool to 0°C, add ice ethanol to the reaction solution, stir and suction filter the reaction solution to obtain the compound of formula (5). Wherein the acylation reaction and the amine aldehyde condensation ring reaction occur simultaneously in the reaction system; the reagents other than raw materials for the acylation reaction include but are not limited to concentrated sulfuric acid, perchloric acid, tetrafluoroboric acid, hydrogen chloride gas and other inorganic acids and benzene Organic acids such ...
Embodiment 2
[0062] Steps a)-d) in this embodiment are similar to steps a)-d) in Embodiment 1, and will not be repeated in this embodiment;
[0063] Step e): the compound of formula (2) generates the compound of formula (1) through decarboxylation reaction; add the compound of formula (2) into the boric acid solution, heat to reflux reaction, cool to room temperature, suction filter the reaction solution, and bake the filter cake After drying the compound of formula (1) is obtained.
[0064] Specifically, in the reaction bottle, put Add 37g (0.1m) into a saturated aqueous solution of boric acid, heat to reflux, react for 30 hours, cool to room temperature, filter the reaction solution with suction, and dry the filter cake to obtain 16g, the yield is 70%; 1H NMR (600MHz, CDCl3): δ8.09(s, 1H), 7.59(s, 1H), 7.43-7.41(m, 2H), 5.79-5.77(m, 2H), 4.96(d,J=6.0Hz,1H),4.91(d,J=6.0Hz,1H),3.13-3.11(m,2H),2.88(d,J=12.0Hz,2H),2.62(d,J =12.0Hz,2H).13C NMR (100MHz,CDCl3):δ155.57,149.32,137.24,137.09,...
Embodiment 3
[0066] Steps a)-d) in this embodiment are similar to steps a)-d) in Embodiment 1, and will not be repeated in this embodiment;
[0067] Step e): the compound of formula (2) generates the compound of formula (1) through decarboxylation reaction; the compound of formula (2) is added in the lithium chloride solution, heated to reflux reaction, cooled to room temperature, suction filtered the reaction solution, filtered The compound of formula (1) is obtained after the cake is dried.
[0068] Specifically, in the reaction bottle, put Add 37g (0.1mol) and 8.5g (0.2mol) of lithium chloride to 200mL of DMSO, heat to 180°C, and react for 10 hours. Pour the reaction solution into ice water. After stirring, a large amount of solids precipitate out. cake after drying 17g, the yield is 74%; 1H NMR (600MHz, CDCl3): δ8.09(s, 1H), 7.59(s, 1H), 7.43-7.41(m, 2H), 5.79-5.77(m, 2H), 4.96(d,J=6.0Hz,1H),4.91(d,J=6.0Hz,1H),3.13-3.11(m,2H), 2.88(d,J=12.0Hz,2H),2.62(d,J =12.0Hz,2H).13C NMR(100MH...
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