- Cobalt-catalyzed direct α-hydroxymethylation of amides with methanol as a C1 source
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Herein, we report a cobalt-catalyzed α-hydroxymethylation of amides with methanol under mild conditions. Using CoCl2·6H2O as an inexpensive and efficient catalyst, some important bioactive β-hydroxyamides were obtained in moderate to excellent yields. The
- Ma, Ben,Sun, Rongxia,Yang, Jingya
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supporting information
p. 1382 - 1385
(2022/02/05)
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- Preparation method of topivacamide
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The invention relates to a preparation method of topivacamide. The method comprises the following steps: (1) adding 3-hydroxy-2-phenylpropionic acid and toluene into a beaker, stirring uniformly, carrying out nitrogen displacement, protecting, and carrying out heating reflux until the mixture is insoluble; respectively adding triethylamine and acetyl chloride in the reaction, heating and refluxinguntil the solution is clear, cooling to room temperature, dropwise adding thionyl chloride, continuously reacting, and concentrating under reduced pressure to obtain 2-chlorocarbonyl-2-phenyl ethyl ester; and (2) preparing another jacketed bottle, adding ethylpyridine-4-ylmethylamine, triethylamine and methylbenzene, replacing with nitrogen, protecting, cooling, and slowly dropwise adding 2-chlorocarbonyl--2phenyl ethyl ester into the methylbenzene solution; after the dripping is finished, continuously reacting; (3) after the reaction is completed, dropwise adding water, carrying out liquid separation extraction, washing with saline water, adding a 3N hydrochloric acid solution into a toluene layer for hydrolysis, cooling to room temperature, carrying out liquid separation, separating toobtain a water phase, and washing with water phase ethyl acetate; (4) cooling, dropwise adding a saturated sodium bicarbonate aqueous solution to adjust the pH value, extracting with ethyl acetate, and concentrating an organic phase to obtain a faint yellow oily matter; and (5) dissolving the oily substance crude product with ethyl acetate, slowly dropwise adding heptane, crystallizing, carrying out suction filtration, and washing to obtain the target product topivacamide.
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Paragraph 0014; 0050-0054
(2021/04/03)
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- Process for preparing N- ethylpyridine methylamine hydrochloride crystal, and application thereof in preparation of itemamide (by machine translation)
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An application N - of,ethylpyridine methylamine hydrochloride crystal, prepared by dissolving N -ethylpyridine methylamine N - in an organic solvent, at room temperature or heating X - in an organic solvent is stirred until the material is completely dissolved, is stirred until the material is completely dissolved or stirred at about 9.73 °, 14.61 °, 17.98 °, 18.49 °, 20.36 °, 24.63 °, 27.21 ° with a diffraction peak, and is stirred. N - through a,ray powder diffractogram, for drying to obtain the supported product amide key starting material, ethyl-pyridine methylamine hydrochloride; is prepared by filtering, and drying. The crystal has the advantages of simple operation, purification effect, crystallization and high N -purity crystal, form impurity content in the, preparation of the itemamide hydrochloride, crystal . and is, simple and convenient, operation. (by machine translation)
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Paragraph 0026
(2020/05/02)
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- N-ethylpyridine methylamine mesylate crystal, preparation process thereof and application of N-ethylpyridine methylamine mesylate crystal in preparation of tropicamide
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The invention discloses an N-ethylpyridine methylamine mesylate crystal, a preparation process thereof and the application of the N-ethylpyridine methylamine mesylate crystal in the preparation of tropicamide. Mesylate of N-ethylpyridine methylamine mesylate crystal is prepared from N-ethylpyridine methylamine and methylsulfonic acid, when X-ray powder diffraction is used, and the crystal has diffraction peaks at about 9.49 degrees, 13.16 degrees, 16.18 degrees, 19.10 degrees, 20.54 degrees, 23.24 degrees, 26.96 degrees and 34.63 degrees. The preparation method comprises the following steps ofdissolving the N-ethylpyridine methylamine in an organic solvent, and stirring at room temperature or heating and stirring until a material is completely dissolved; slowly adding acid, and crystallizing; and carrying out heat preservation aging, filtering and drying to obtain the tropicamide key starting material N-ethylpyridine methylamine mesylate crystal. The method is simple to operate and obvious in purification effect, the salt form impurity content and the crystal form impurity content prepared by crystallization are low, the purity is high, and the industrial production is facilitated.
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Paragraph 0025
(2020/04/17)
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- N- Ethylpyridine methylamine hydrochloride and crystal, preparation process and application thereof
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The invention discloses N -ethyl-pyridine methylamine trifluoroacetate, and a crystal. preparation process and application N - thereof to prepare N -ethylpyridine methylamine hydrochloride crystals, by slowly adding X -ethyl-pyridine methylamine, in an organic solvent 15.12 °, 15.45 °, 17.68 °, 20.68 °, 22.62 °, 23.25 °, 24.75 °, 29.54 ° at room temperature or heating. to fully dissolve N -ethyl-pyridine methylamine . through heating for, hours to prepare the ethyl-pyridine methylamine trifluoroacetate crystals . The method is simple in operation and;% in crystal form impurity content, obtained by dry-adding trifluoroacetic acid; crystals, at about, at room temperature or, in a heating mode of heating the crystals at a temperature ranging from, N - degrees, to a. material completely-dissolving solution.
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- Synthetic method of tropicamide
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The invention relates to a production method of chemical medicines and particularly relates to a synthetic method of tropicamide. The synthetic method comprises the steps of carrying out hydrolysis and acylation on the raw material, namely diethyl phenylmalonate, condensing diethyl phenylmalonate with N-ethyl-4-methylpyridine amine, and generating reduction reaction with hydroboron, so as to obtain tropicamide. The synthetic method has the beneficial effects that the raw material cost is low, the properties of an intermediate product are stable, impurities are few, the operation steps such aspurification are reduced, and the process is simplified; reaction conditions are safe and mild, extremely toxic substances are not introduced, and the industrial amplified production is promoted; andby optimizing the raw material ratio, the total yield of the reaction is increased to be 65% and is greatly increased, and the production cost is lowered.
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Paragraph 0062; 0067; 0072; 0077; 0082
(2018/03/24)
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- Thiazolidinone, oxazolidinone, and imidazolone derivatives for treating non-inflammatory gastrointestinal tract disorders
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A method is provided for using Cav2.2 subunit calcium channel modulators, particularly thiazolidinone, oxazolidinone, and imidazolone derivatives, to treat non-inflammatory gastrointestinal tract disorders.
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