A kind of preparation method of sodium phenylbutyrate
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A sodium phenylbutyrate preparation technology, which is applied in the field of preparation of sodium phenylbutyrate, can solve the problems of low product yield, many synthesis steps, complicated post-treatment purification process, etc.
Active Publication Date: 2021-09-10
NANJING TECH UNIV
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[0003] However, in the existing synthetic method of sodium phenylbutyrate, there are generally many synthetic steps, poor reaction regioselectivity, low product yield, and the reaction conditions are not mild, and the reaction and post-treatment purification process are relatively complicated.
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Embodiment 1
[0018] (1) Under an argon atmosphere, add the material and anhydrous 2,3-butanediol in a molar volume ratio of 0.1mmol:0.1mL to the reaction vessel and mix well; wherein, the related materials include a molar ratio of 1: 3:0.01:0.2:5:3:100 of N-(octaaminoquinoline)but-3-enamide, bromobenzene, allylpalladium(II) chloride dimer, 2-(dicyclohexylphosphine Acyl)-1-phenyl-1H-pyrrole, lithium acetate, cyanoacetic acid and water;
[0019] (2) Place the reaction vessel in an oil bath at 125°C and vigorously stir for 12 hours, and purify the reaction product through a silica gel column (flush the chromatography silica gel column with petroleum ether at a ratio of 1:20 to ethyl acetate), to obtain The compound is determined to be 4-phenyl-N-(quinolin-8-yl)butanamide through detection.
Embodiment 2
[0021] This embodiment is basically the same as Embodiment 1, the difference is:
[0022] In step (1), N-(octaaminoquinoline)but-3-enamide, bromobenzene, allylpalladium(II) chloride dimer, 2-(dicyclohexylphosphono)-1- The molar ratio of phenyl-1H-pyrrole, lithium acetate, cyanoacetic acid and water is 1:1:0.1:0.02:1:1:1;
[0023] In step (2), the temperature of the oil bath is 130°C.
Embodiment 3
[0025] This embodiment is basically the same as Embodiment 1, the difference is:
[0026] In step (1), N-(octaaminoquinoline)but-3-enamide, bromobenzene, allylpalladium(II) chloride dimer, 2-(dicyclohexylphosphono)-1- The molar ratio of phenyl-1H-pyrrole, lithium acetate, cyanoacetic acid and water is 1:2:0.05:0.1:3:2:50;
[0027] In step (2), the temperature of the oil bath is 135°C.
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Abstract
The invention discloses a preparation method of sodium phenylbutyrate. In the present invention, under an inert atmosphere, materials and anhydrous 2,3-butanediol are added to the reaction vessel and mixed; the related materials include allyl palladium chloride (II) dimer, 2-( Cyclohexylphosphono)-1-phenyl-1H-pyrrole, N-(octaminoquinoline) but-3-enamide, lithium acetate, bromobenzene, cyanoacetic acid and water; place the reaction vessel at 125-135°C The reaction was stirred vigorously in an oil bath for 12 hours, and the reaction product was purified through a silica gel column to obtain a compound with a directing group; the compound was added to an ethanol solvent containing sodium hydroxide, and the mixture was heated to 130-140°C for reflux reaction After 12 hours, the reaction product was distilled under reduced pressure to remove the solvent, extracted, collected the water layer, and removed the water by distillation under reduced pressure to obtain a sodium phenylbutyrate preparation. The invention has the characteristics of high reaction region selectivity and high yield, mild reaction conditions, and simple reaction and post-treatment purification process.
Description
technical field [0001] The invention belongs to the technical field of organic chemistry, in particular to a preparation method of sodium phenylbutyrate. Background technique [0002] Sodium phenylbutyrate is a prodrug that is rapidly metabolized to phenylacetate. It can be combined with glutamic acid and ammonia to form phenylacetylglutamine, which is excreted through the kidneys, which is another way for nitrogenous waste to be excreted. Taking sodium phenylbutyrate can reduce the high blood ammonia level and blood glutamic acid concentration, and increase the excretion of nitrogenous waste in the form of phenylacetyl glutamine. It is suitable for all neonatal enzyme deficiency (complete enzyme deficiency within 28 days after birth), delayed enzyme deficiency (partial enzyme deficiency after the first month of life) with a family history of hyperammonemic encephalopathy . [0003] However, in the existing synthetic method of sodium phenylbutyrate, there are generally ma...
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