- Efficient synthesis, X-ray diffraction study and antimicrobial activity of some novel thiazolidin-4-ones and perhydro-1,3-thiazin-4-ones
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Condensations of thiosemicarbazones 1 derived from 1-tetralones with chloroacetic acid and 2-bromopropionic acid in the presence of N -methylpyridinium p -toluenesulfonate (an ionic liquid) yield the corresponding 2-substituted 4-thiazolidinones 2. The re
- Gautam, Deepika,Gautam, Poonam,Chaudhary, Ram P.
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- Method for preparing (S)-2-[3-(3-fluorobenzyl)-4-(3-fluorobenzyloxy)benzylamino]propionamide and salts thereof
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The invention relates to a method for preparing (S)-2-[3-(3-fluorobenzyl)-4-(3-fluorobenzyloxy)benzylamino]propionamide and salts thereof. Salts of (S)-2-[3-(3-fluorobenzyl)-4-(3-fluorobenzyloxy)benzylamino]propionamide mean (S)-2-[3-(3-fluorobenzyl)-4-(3-fluorobenzyloxy)benzylamino]propionamide mesylates. The preparation method comprises the step of preparing the target product through synthesizing novel compounds, i.e., 2-(3-bromo-4((3-fluorobenzyl)oxy)phenyl)-1,3-dioxolane and 2-((3-fluorobenzyl)oxy)-5-formyl phenylboronic acid and belongs to bran-new preparation methods. The yield of the (S)-2-[3-(3-fluorobenzyl)-4-(3-fluorobenzyloxy)benzylamino]propionamide prepared by the preparation method is 49.57%, and the HPLC purity reaches 78.92%, and the yield of the salts of the prepared (S)-2-[3-(3-fluorobenzyl)-4-(3-fluorobenzyloxy)benzylamino]propionamide is 50.40%, and the HPLC purity reaches 96.35%, so that the yield and the HPLC purity are improved greatly compared with those in the prior art.
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Paragraph 0072-0075
(2017/05/12)
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- Preparation method of 3-(3-luorobenzyl)-4-(3-fluorobenzyloxy)benzaldehyde
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The invention relates to a preparation method of 3-(3-luorobenzyl)-4-(3-fluorobenzyloxy)benzaldehyde. The preparation method comprises the following steps: respectively preparing 3-bromo-4-[(3-fluorobenzyl)oxy]benzaldehyde and pyridinium p-toluenesulfonate, letting 3-bromo-4-[(3-fluorobenzyl)oxy]benzaldehyde react with pyridinium p-toluenesulfonate to generate 2-(3-bromo-4-((3-fluorobenzyl)oxy)phenyl)-1,3-dioxolame, hydroxylating 2-(3-bromo-4-((3-fluorobenzyl)oxy)phenyl)-1,3-dioxolame to obtain 2-((3-fluorobenzyl)oxy)-5-formylphenylboronic acid, and finally coupling 2-((3-fluorobenzyl)oxy)-5-formylphenylboronic acid and m-fluorobenzyl bromide to obtain the target product. The invention provides a method for directly preparing 3-(3-luorobenzyl)-4-(3-fluorobenzyloxy)benzaldehyde. By the method, yield of the 3-(3-luorobenzyl)-4-(3-fluorobenzyloxy)benzaldehyde reaches up to 64.85%, and purity measured by high performance liquid chromatography reaches 98.92%.
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Paragraph 0065; 0066; 0067
(2017/08/28)
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- 2-(3-bromine-4-(3-fluorobenzyloxy)phenyl)-1,3-dioxolame and preparation method thereof
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The invention relates to a new compound 2-(3-bromine-4-(3-fluorobenzyloxy) phenyl)-1,3-dioxolame and a preparation method thereof. The preparation method includes: respectively preparing 3-bromine-4-(3-fluorobenzyloxy) benzaldehyde and 4-methyl benzenesulfonic acid pyridinium first, and allowing the 3-bromine-4-(3-fluorobenzyloxy) benzaldehyde to have reaction with the 4-methyl benzenesulfonic acid pyridinium to generate the 2-(3-bromine-4-(3-fluorobenzyloxy) phenyl)-1,3-dioxolame. The 2-(3-bromine-4-(3-fluorobenzyloxy) phenyl)-1,3-dioxolame prepared by the method can be directly used for preparing 3-(3-fluorobenzyl)-4-(3-fluorobenzyloxy) benzaldehyde, the yield of the prepared 3-(3-fluorobenzyl)-4-(3-fluorobenzyloxy) benzaldehyde reaches up to 64.85%, and the purity, measured by high performance liquid chromatography, of the 3-(3-fluorobenzyl)-4-(3-fluorobenzyloxy) benzaldehyde reaches 98.92%.
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Paragraph 0069; 0070; 0071
(2017/08/29)
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- 2-(3-fluorobenzyloxy)-5-formylphenylboronic acid and preparation method thereof
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The invention relates to a novel compound, i.e., 2-(3-fluorobenzyloxy)-5-formylphenylboronic acid and a preparation method thereof. The method comprises the steps of firstly, separately preparing 3-bromo-4-[(3-fluorobenzyl)oxy]phenylaldehyde (represented by a formula 3) and 4-toluenesulfonic acid pyridinium (represented by a formula 6), then, enabling the compound represented by the formula 3 and the compound represented by the formula 6 to react so as to produce 2-(3-bromo-4-(3-fluorobenzyloxy)phenyl)-1,3-dioxolane (represented by a formula 7), and enabling the compound represented by the formula 7 to make a coupling reaction, thereby obtaining 2-(3-fluorobenzyloxy)-5-formylphenylboronic acid (represented by a formula 8). The novel compound, i.e., 2-(3-fluorobenzyloxy)-5-formylphenylboronic acid provided by the invention can be used for preparing 3-(3-fluorobenzyl)-4-(3-fluorobenzyloxy)phenylaldehyde, the yield of the prepared 3-(3-fluorobenzyl)-4-(3-fluorobenzyloxy)phenylaldehyde reaches 64.85%, and the purity measured through high-performance liquid chromatography at least reaches 98.92%.
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Paragraph 0073; 0074; 0075
(2017/08/27)
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- Esterification catalysis by pyridinium p -toluenesulfonate revisited - Modification with a lipid chain for improved activities and selectivities
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The lipid analogs of pyridinium p-toluenesulfonate (PPTS) were examined for catalysis of the condensation of an equimolar mixture of carboxylic acids and alcohols under mild conditions without removal of water. Although PPTS is a poor catalyst, the introduction of a lipid chain and nitro group significantly improved the activity of PPTS and led to selectivity at suppressing the elimination side reactions of alcohols. 2-Oleamido-5-nitro-pyridinium p-toluenesulfonate (6) is a lead catalyst that promoted various esterification reactions with yields up to 99%.
- Wang, Wei,Liu, Huimin,Xu, Shaoyi,Gao, Yong
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supporting information
p. 2906 - 2912
(2013/09/02)
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- Vitamin d analogues
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Compounds of the formula I wherein X represents hydrogen or hydroxy; R1 and R2, which may be the same or different, represent hydrogen, (C1-C4)alkyl optionally substituted with one hydroxyl group or one or more fluorine atoms, or, together with the carbon atom to which they are attached, R1 and R2 form a (C3-C5)carbocyclic ring; R3 represents (C1-C4)alkyl, (C1-C4)alkoxy or a halogen atom, such as fluorine, chlorine, bromine, or iodine, and in-vivo hydrolyzable esters thereof with pharmaceutically acceptable acids, may be used in the prophylaxis and/or treatment of dieases characterized by abnormal cell differentiation and/or cell proliferation.
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- Process for producing simvastatin
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This invention provides an easy and efficient process for producing a simvastatin of great use as an HMG-CoA reductase inhibitor, which comprises deacylation of lovastatin with an inorganic base and a secondary or tertiary alcohol and subjecting the resulting diol lactone to selective protection with a ketal or acetal protective group, acylation and deprotection-lactonization to give simvastatin.
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- PROTEASE-BINDING COMPOUNDS AND METHODS OF USE
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Non-peptide, protease-binding compounds are described as useful in the detection, labelling, and inhibition of retroviral proteases. Aryl piperidinyl derivatives and other compounds related in structure have been found to be HIV-1 and HIV-2 protease-binding compounds.
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- Prostaglandin E1 analogues
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A prostaglandin E1 analogue represented by formula STR1 wherein R1 represents a hydrogen atom or a C1 -C6 alkyl group; and X is an oxygen atom and R2 represents STR2 or X is a sulfur atom and R2 represents STR3 The compound has a strong and prolonged inhibitory action for platelet aggregation and is useful for treatment of various thrombotic diseases including peripheral circulatory disturbance.
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- Vitamin D compound, method of preparing this compound and intermediate thereof
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The invention relates to a new vitamin D compound, substituted in the 18-position with an alkyl group, a hydroxy group, an alkoxy group, an alkenyl group, an alkynyl group, a fluorinated alkyl group or a fluorinated alkenyl group. The invention also relates to a method of preparing said vitamin D compound and to a lactone and a hydrindane intermediate. The vitamin D compound is of the general formula STR1
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- Electron beam-graftable compound and product from its use
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A compound of the formula: STR1 in which: (a) each of A and B independently is phenyl which may be unsubstituted or substituted; (b) each of R1 and R2 independently is hydrogen or C1 -C6 alkyl; (c) m represents an integer of from 0 to about 18; and (d) Z is poly(alkyleneoxy) which may be uncapped or capped with a C1 -C6 alkyl group. The compound can be grafted to polyolefin nonwoven webs by electron beam radiation without significant homopolymerization. The grafted webs are wettable (hydrophilic) and capable of withstanding multiple rewets without substantial removal of grafted compound. The grafted webs are especially well-suited for use in disposable absorbent products.
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