- Method for removing and recovering impurities in methoxylamine hydrochloride synthesis reaction raw material
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The invention provides a method for removing and recovering impurities in a methoxylamine hydrochloride synthesis reaction raw material, which belongs to the field of chemical engineering. The methodcomprises the following steps: (1) removal: adding an alkaline reagent into the methoxylamine hydrochloride synthesis reaction raw material, mixing, and separating methyl-removed impurities on one side; and (2) recovery: adding a methylation reagent into the methyl-removed impurities on one side separated in the step (1) to carry out a methylation reaction so as to obtain 2, 5-dimethoxypropiophenone, and recovering the 2, 5-dimethoxypropiophenone. According to the method, the characteristic that phenolic hydroxyl groups in impurities of a methoxylamine hydrochloride synthesis reaction raw material are weakly acidic is utilized, and the alkaline reagent is added to react with methyl-removed impurities on one side to form corresponding salt separation, so that impurities in the raw material2, 5-dimethoxypropiophenone are removed; after the separated impurity sodium salt is methylated again, 2, 5-dimethoxypropiophenone can be obtained again and recycled. The method is simpler and more convenient to operate, high in impurity removal rate and capable of effectively increasing the utilization rate of impurities in raw materials.
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Paragraph 0018-0020; 0022-0023; 0025; 0027
(2021/01/28)
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- 3-Ylidenephthalides as a new class of transient receptor potential channel TRPA1 and TRPM8 modulators
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Following the recent identification of the naturally occurring 3-ylidene-4,5-dihydrophthalide ligustilide and its oxidation product dehydroligustilide as novel TRPA1 modulators, a series of seventeen 3-ylidenephthalides was synthesized and tested on TRPA1 and TRPM8 channels. Most of these compounds acted as strong modulators of the two channel types with EC50 and/or IC50 values distinctly lower than those of the reference compounds.
- Ortar, Giorgio,Schiano Moriello, Aniello,Morera, Enrico,Nalli, Marianna,Di Marzo, Vincenzo,De Petrocellis, Luciano
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p. 5614 - 5618
(2013/10/01)
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- Probes for narcotic receptor mediated phenomena. 39. Enantiomeric n-substituted benzofuro[2,3-c]pyridin-6-ols: synthesis and topological relationship to oxide-bridged phenylmorphans
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Enantiomers of N-substituted benzofuro[2,3-c]pyridin-6-ols have been synthesized, and the subnanomolar affinity and potent agonist activity of the known racemicN-phenethyl substituted benzofuro[2,3-c]pyridin-6-ol can now be ascribed to the 4aS,9aRenantiomer. The energy-minimized structures suggest that the active enantiomer bears a greater three-dimensional resemblance to morphine than to an ostensibly structurally similar oxide-bridged phenylmorphan. Structural features of the conformers of N-substituted benzofuro[2,3-c]pyridin- 6-ols were compared to provide the rationale for their binding affinity.
- Zhang, Yi,Lee, Yong Sok,Rothman, Richard B.,Dersch, Christina M.,Deschamps, Jeffrey R.,Jacobson, Arthur E.,Rice, Kenner C.
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experimental part
p. 7570 - 7579
(2010/05/18)
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- Studies on the Friedel-Crafts Reaction. XVI, Preparation of Isomeric 2-Acyl- and 3-Acyl-4-methoxy Phenols
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Acylation of 4-methoxy phenol according to Friedel and Crafts, as well as the rearrangement of its esters according to Fries lead always to 2-acyl-4-methoxy phenols or to their demethylated compounds.The unknown 3-acyl-4-methoxyphenols were prepared in two steps: First, the ester is acylated with the corresponding acyl chloride and SnCl4 in nitromethane.In the second step the resulting ketoesters are hydrolysed.This is a general method.The yields of meta-acylphenols are between 40 and 90percent.The isomeric 2-acyl-4-methoxyphenols which were partly unknown or accessible only in low yields have also been prepared for comparative spectral studies (UV, IR, NMR, MS) of ortho- and meta-acylphenols. - Keywords: Friedel-Crafts acylation; Fries rearrangement; Ketoesters; Spectral data
- Martin, Robert
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p. 1155 - 1164
(2007/10/02)
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- Psychotomimetic phenylisopropylamines. 5. 4 alkyl 2,5 dimethoxyphenylisopropylamines
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A homologous series of 4 alkyl 2,5 dimethoxyphenylisopropylamines (alkyl = H through n C5H11 and t C4H9) was synthesized and compared with mescaline as serotonin agonists in a sheep umbilical preparation. The three carbon homolog 6d was found to be the most potent of the straight chain series in accordance with its observed psychotomimetic effectiveness in man.
- Shulgin,Dyer
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p. 1201 - 1204
(2007/10/06)
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