- A 4 - amino -3 - fluoro phenol high efficient synthesis method (by machine translation)
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The invention discloses a 4 - amino - 3 - fluoro phenol high efficient synthesis method, specifically comprises the following steps: first preparing porous polystyrene micro-ball, and then added to the hydrolysate of titanium tetrachloride, the reaction is carried out under certain conditions to make the supported catalyst, finally a pair of nitro phenol as raw materials to make the 3 - fluoro - - 4 nitro phenol, then in the above prepared under the catalysis of the supported catalyst, dropping the sodium borohydride solution reaction, to obtain the target product. The method is simple in operation, the equipment requirement is low, the yield is high. (by machine translation)
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Page/Page column 4; 5; 6; 7
(2019/01/05)
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- Synthesis method of intermediate 3-fluoro-4-nitrophenol
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The invention discloses a synthesis method of intermediate 3-fluoro-4-nitrophenol. The method comprises steps as follows: (1) 2,4-dibromonitrobenzene and water are mixed, the mixture is heated to 50-60 DEG C, cobalt acetate is added under the protection of inert gas, the mixture is stirred and mixed uniformly, ammonia water is dropwise added, the mixture is subjected to a reflux reaction and continuously stirred for a reflux reaction for 1-2 h after ammonia water is dropwise added, centrifugation and separation are performed after the reaction is completed, an organic phase is collected, reduced pressure distillation is performed, a mixture of 3-bromo-4-nitrophenol and 5-nitrophenol-2-nitrophenol is prepared, and 3-bromo-4-nitrophenol is prepared through water steam distillation, ether extraction, recrystallization and isomeride separation; (2) 3-bromo-4-nitrophenol is added to DMSO, polyethylene glycol-400 is added, the mixture is stirred and mixed uniformly and then heated to 40-50 DEG C, potassium fluoride is added, the mixture is stirred for a reaction for 4-5 h, reduced pressure distillation is performed after the reaction ends, and 3-fluoro-4-nitrophenol is prepared through recrystallization. The synthesis method is simple to operate and mild in condition, fewer by-products are produced, the product purity is high and the product yield is higher.
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Paragraph 0022; 0029; 0036; 0038; 0043; 0050
(2018/05/16)
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- 4-amino-3-fluorophenol and synthesizing method thereof
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The invention discloses 4-amino-3-fluorophenol and a synthesizing method thereof.The synthesizing method comprises the steps that fluoroaniline serves as a raw material, a diazo-reaction is carried out first, then a fluorine resolving reaction is carried out, and a white diazonium salt solid is obtained; then, the white diazonium salt solid is subjected to a hydrolysis reaction, and 3-fluorophenol is obtained; 3-fluorophenol is then subjected to a nitration reaction, and 3-fluorine-4-nitrophenol is obtained; then, obtained 3-fluorine-4-nitrophenol is reduced, and 4-amino-3-fluorophenol is obtained.According to 4-amino-3-fluorophenol and the synthesizing method thereof, ionic liquid serves as a reaction solvent, the volatility is low, environment is easily protected, and no harm is caused to the human body; in the reaction of reducing nitro groups into amino groups, the microwave heating mode is adopted, so that the reaction efficiency is greatly improved, and the product yield is increased.
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Paragraph 0020; 0023
(2016/10/10)
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- Method for synthesizing 3-fluoro-4-aminophenol
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The invention provides a method for synthesizing 3-fluoro-4-aminophenol. The method comprises the following steps: (1) preparing a composite catalyst from nickel nitrate, palladium chloride and butyl titanate through a sol-gel method; (2) enabling metallic sodium and 2,4-difluoronitrobenzene and methanol to react so as to prepare 2-fluoro-4-methoxyl-nitrobenzene; (3) performing a demethylation reaction on 2-fluoro-4-methoxyl-nitrobenzene through aluminum chloride so as to prepare 3-fluoro-4-nitrophenol; (4) performing a catalytic hydrogenation reaction on the 3-fluoro-4-nitrophenol by using a composite catalyst, thereby obtaining 3-fluoro-4-aminophenol. The method is relatively high in yield, and the product is also relatively high in purity.
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Paragraph 0045
(2017/02/09)
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- Probing synergy between two catalytic strategies in the glycoside hydrolase O-GlcNAcase using multiple linear free energy relationships
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Human O-GlcNAcase plays an important role in regulating the post-translational modification of serine and threonine residues with β-O-linked N-acetylglucosamine monosaccharide unit (O-GlcNAc). The mechanism of O-GlcNAcase involves nucleophilic participation of the 2-acetamido group of the substrate to displace a glycosidically linked leaving group. The tolerance of this enzyme for variation in substrate structure has enabled us to characterize O-GlcNAcase transition states using several series of substrates to generate multiple simultaneous free-energy relationships. Patterns revealing changes in mechanism, transition state, and rate-determining step upon concomitant variation of both nucleophilic strength and leaving group abilities are observed. The observed changes in mechanism reflect the roles played by the enzymic general acid and the catalytic nucleophile. Significantly, these results illustrate how the enzyme synergistically harnesses both modes of catalysis; a feature that eludes many small molecule models of catalysis. These studies also suggest the kinetic significance of an oxocarbenium ion intermediate in the O-GlcNAcase-catalyzed hydrolysis of glucosaminides, probing the limits of what may be learned using nonatomistic investigations of enzymic transition-state structure and offering general insights into how the superfamily of retaining glycoside hydrolases act as efficient catalysts.
- Greig, Ian R.,Macauley, Matthew S.,Williams, Ian H.,Vocadlo, David J.
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supporting information; experimental part
p. 13415 - 13422
(2010/01/16)
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- USE OF INTERMEDIATES ((R ) -2,2, 4-TRIMETHYL-L, 3-DIOXOLANE-4-YL) METHANOL (A), 3-F LUORO-4-NITRO-PHENOL (B) AND 1- (4-CHLORO- BENZYL) -PIPERIDIN-4-YLAMINE (C)
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The present invention relates to novel processes for the preparation of intermediate compounds which can be used to prepare therapeutic agents. The present invention also relates to novel intermediate compounds which can be used to prepare therapeutic agents. More specifically, the invention relates to the use of intermediates ((R) -2,2,4-trimethyl-l, 3- dioxolane-4 -yl) methanol (A), 3-f luoro-4-nitro-phenol (B) and 1- (4-chloro-benZyl) -piperidin-4-ylamine (C).
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Page/Page column 8; 19-20
(2009/04/25)
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- NOVEL PROCESS I
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The present invention relates to a novel process for the preparation of compounds of Formula (I) wherein X, Q, R1 and R2 are as defined in the specification, the compounds being useful in the preparation of therapeutic agents. The invention further relates to novel intermediates useful in the preparation of the therapeutic agents.
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Page/Page column 35-36
(2008/06/13)
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- Aniline derivatives having herbicidal activity, their preparation and their use
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Compounds of formula (I): STR1 (wherein: R1 is optionally substituted alkyl, cycloalkyl, optionally substituted alkoxy, or optionally substituted alkylthio; R2 is hydrogen, optionally substituted alkyl, cycloalkyl, optionally substituted alkenyl, optionally substituted alkynyl or a group of formula --YR7 ; R3 is optionally substituted alkyl, cycloalkyl, optionally substituted alkoxy group, optionally substituted alkenyl, optionally substituted alkynyl, halogen, nitro or a group of formula --COR8, wherein R8 is hydrogen, alkyl, cycloalkyl or alkoxy; R4 and R5 are each hydrogen atom or alkyl; R6 is optionally substituted alkyl, cycloalkyl, optionally substituted alkoxy group, optionally substituted alkenyl, optionally substituted alkynyl, halogen, nitro, or a group of formula --COR8, as defined above; A, Q and X are each oxygen or sulfur; Y is a group of formula --CO--, --COO--, --CH2 O--, --CH2 S--, --CH2 CH2 O--, --CH2 CH2 S--, --CH2 CO--, --CH2 COO--, --CH(Me)COO--, --CH2 CH2 CO--, --CH2 OCO--, CH2 OCOO-- and --CH2 CH2 OCO--; R7 is optionally substituted alkyl group, cycloalkyl, optionally substituted alkenyl, optionally substituted alkynyl, optionally substituted aryl, optionally substituted aralkyl, or an optionally substituted heterocycle; and m and n are each an integer from 0 to 4; and herbicidally acceptable addition salts thereof) are useful as herbicides.
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- SYNTHESIS AND BIOLOGICAL ACTIVITY OF NOVEL N-1-ARYL-6-FLUORO-5-METHYL-1,8-NAPHTHYRIDINE-3-CARBOXYLIC ACIDS
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A series of 5-methyl-4-oxo-1,8-naphthyridine-3-carboxylic acids was prepared in which the N-1 position was substituted by various aryl groups.Seven compounds showed excellent in vitro antibacterial activity against Gram-positive and Gram-negative strains.
- Jacquet, Jean-Pierre,Bouzard, Daniel,Cesare, Pierre Di,Dolnic, Nicolas,Massoudi, Massoud,Remuzon, Philippe
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p. 2301 - 2311
(2007/10/02)
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