19 results about "Phenylcarbamates" patented technology

The invention relates to the field of organic compound synthesis, and more particularly to the production of valuable compounds for use in organic synthesis, and even more particularly to a method of producing O-methyl-N-phenyl carbamate of the formula shown. What is proposed is a method of producing O-methyl-N-phenyl carbamate of the given formula, which comprises reacting methanol with diphenylurea, wherein methanol is reacted with diphenylurea at a molar ratio of the reagents diphenylurea:methanol of 1:(6-15), and the process is carried out at a temperature of from 120 to 190°C to produce 99.9% pure O-methyl-N-phenyl carbamate, with subsequent separation of the products of the process by fractionation. The technical result of the proposed invention is an improved method of producing O-methyl-N-phenyl carbamate under optimal process conditions with a yield of 78-89% and separation of the products of the process by fractionation.

The invention relates to a novel method of producing 4,4'-methylene diphenyl diisocyanate (MDI). A phosgene-free method of producing 4,4'-methylene diphenyl diisocyanate is characterized in that diphenylurea is produced from urea and aniline in an aromatic hydrocarbon medium, and the resulting diphenylurea is reacted with an excess of methanol to produce O-methyl-N-phenyl carbamate; molten O-methyl-N-phenyl carbamate is reacted with anhydrous derivatives of formaldehyde in the presence of acidic catalysts to produce 4,4'-methylene diphenyl dicarbamate; 4,4'-methylene diphenyl dicarbamate in the form of a melt, or of a suspension in an inert carrier liquid, or of a powder is subjected to continuous thermal decomposition in a stream of inert gas, and 4,4'-methylene diphenyl diisocyanate is isolated by fractionation. The invention provides a novel phosgene-free method of synthesizing 4,4'-MDI, which is suitable for industrial-scale implementation.

The invention discloses an HPLC (High Performance Liquid Chromatography) detection method for ipragmine hydrochloride enantiomers, and belongs to the technical field of pharmaceutical analysis. The HPLC detection method provided by the invention comprises the following steps: dissolving ipragmine hydrochloride to be detected in a diluent to prepare a test solution; detecting the test solution by adopting normal-phase high performance liquid chromatography; the stationary phase of the normal-phase high performance liquid chromatography is silica gel of which the surface is covalently bonded with cellulose-tri (3-chloro-4-methyl phenyl carbamate); a mobile phase of the normal-phase high performance liquid chromatography is a mixed solution of normal hexane, isopropanol, trifluoroacetic acid and diethylamine. According to the detection method established by the invention, the ipragmine hydrochloride main peak and the S-configuration enantiomer impurity peak can be subjected to baseline separation, the separation degree can reach 4.5 or above, the method is high in specificity and sensitivity, and various methodology verification parameters all meet the drug quality control requirements.

The invention relates to a separation and detection method of oxopyrrolidine compounds and isomers thereof, and belongs to the technical field of pharmaceutical analysis. The separation and detection method comprises the following steps: adopting a high performance liquid chromatography; cellulose-tri-(4-methyl benzoate), cellulose-tri-(halogenated methyl phenyl carbamate), cellulose-tri-(4-chloro-3-methyl phenyl carbamate), amylose-tri-((s)-alpha-methyl benzyl carbamate) and amylose-tri-(3-(4, 5-dichlorophenyl carbamate) are bonded through covalent bonds, and cellulose-tri-(4-methyl benzoate), cellulose-tri-(halogenated methyl phenyl carbamate), cellulose-tri-(4-chloro-3-methyl phenyl carbamate), cellulose-tri-((S)-alpha-methyl benzyl carbamate) and cellulose-tri-(4-chloro-3-methyl phenyl carbamate) are bonded through covalent bonds. A chromatographic column which takes amylose-tri (3-chloro-4-methylphenylcarbamate) covalently bonded on the surface of silica gel as a filler is a separation chromatographic column; a chromatographic column which takes amylose-tri (3-chloro-4-methylphenylcarbamate) or silica gel covalently bonded on the surface of the silica gel as a filler is a separation chromatographic column; and eluting by taking a mixed solution of normal hexane and ethanol as a mobile phase. The method is high in separation degree, high in sensitivity and good in peak pattern.

The invention discloses an analysis method of phenylephrine hydrochloride isomers. Analysis conditions of the method are as follows: a chromatographic column is a chiral chromatographic column bonded with phenyl carbamate beta-cyclodextrin, Chiral CD-Ph, 4.6 mm * 25 cm, 5 [mu] m; a mobile phase is formed by mixing 1% triethylamine-methanol mixed liquid with the ratio of 30: 70 and acetonitrile according to the ratio of 95: 5; the flow velocity is 0.4 to 0.6 mL / min; the column temperature is 38-42 DEG C; the detection wavelength is 220nm. According to the analysis method, phenylephrine hydrochloride and isomers thereof can be rapidly and accurately separated and detected, the analysis efficiency and accuracy are improved, and the analysis cost is reduced.

The invention relates to a detection method of a morphonidazole isomer. The method is a high performance liquid chromatography method, a chromatographic column with amylose-tri (3-chloro-5-methyl phenyl carbamate) covalently bonded on the surface of silica gel as a filler is adopted, a mobile phase A is a 0.05 mol / L monopotassium phosphate solution, the pH value is adjusted to 2.0 + / -0.5 with phosphoric acid, a mobile phase B is acetonitrile, and the mobile phase A and the mobile phase B are subjected to isocratic elution according to the volume ratio of (20-30): (80-70). The detection method provided by the invention is simple and convenient to operate, can effectively separate R and S isomers of morphonidazole, and can accurately determine the content of the isomers.

The invention provides a method for detecting enantiomers of thiamphenicol glycine ester hydrochloride or thiamphenicol glycine ester hydrochloride in a preparation thereof. The method comprises the following steps: preparing a test solution: taking thiamphenicol glycine ester hydrochloride or a preparation thereof to prepare a test solution; chromatographic conditions: adopting chiral chromatography with cellulose tris-(4-chloro-3-methylphenylcarbamate) as a stationary phase and n-hexane:methanol:anhydrous ethanol:trifluoroacetic acid:ethanolamine as a mobile phase; and a determination method: taking the test solution and injecting it into a liquid chromatograph for determination.

A process for obtaining {{6-[(diethylamino)methyl]naphthalen-2-yl}methyl [4-(hydroxycarbamoyl)phenyl]carbamate and / or pharmaceutically acceptable salts thereof having high purity is described. This process allows to obtain a product having an amount of any single unknown impurity equal to or less than 0.10%, as well as a product having a purity greater than 99.5%, preferably equal to or greater than 99.6%.An HPLC method for determining the purity of the product and possible impurities thereof is also described.

Solid forms of (3aR)-1, 3a, 8-trimethyl-1, 2, 3, 3a, 8, 8a-hexahydropyrrolo (2, 3-b) indol- 5-yl phenyl-carbamate tartrate, including crystalline (3aR)-l, 3a, 8-trimethyl-1, 2, 3, 3a, 8, 8a- hexahydropyrrolo (2, 3-b) indol-5-yl phenyl-carbamate tartrate (posiphen D-tartrate Form A), crystalline (3aR)-1, 3a, 8-trimethyl-1, 2, 3, 3a, 8, 8a-hexahydropyrrolo (2, 3-b) indol-5-yl phenyl- carbamate tartrate dihydrate (posiphen D-tartrate Form B), crystalline (3aR)-1, 3a, 8-trimethyl-1, 2, 3, 3a, 8, 8a-hexahydropyrrolo (2, 3-b) indol-5-yl phenyl-carbamate tartrate Form A having the peak of Pattern C (posiphen D-tartrate Form A+Pattem C), and amorphous (3aR)-1, 3a, 8- trimethyl-1, 2, 3, 3a, 8, 8a-hexahydropyrrolo (2, 3-b) indol-5-yl phenyl-carbamate tartrate, are disclosed. Pharmaceutical compositions comprising posiphen D-tartrate Form A, posiphen D- tartrate Form B, posiphen D-tartrate Form A having the peaks of Pattern C, and amorphous posiphen D-tartrate, and methods of treating various conditions by administering these solid forms, are also disclosed.

Disclosed are solid forms of (3aR)-1, 3a, 8-trimethyl-1, 2, 3, 3a, 8, 8a-hexahydropyrrolo (2, 3-b) indol-5-yl phenyl carbamate tartrate, including crystalline (3aR)-1, 3a, 8-trimethyl-1, 2, 3, 3a, 8, 8a-hexahydropyrrolo (2, 3-b) indol-5-yl phenyl carbamate tartrate (Fenicillin D-tartrate Form A), crystalline (3aR)-1, 3a, 8-trimethyl-1, 2, 3, 3a, 8, 8a-hexahydropyrrolo (2, 3-b) indol-5-yl phenyl carbamate tartrate (Fenicillin D-tartrate Form B), crystalline (3aR)-1, 3a, 8- The present invention relates to a (3aR)-1, 3a, 8-trimethyl-1, 2, 3, 3-b) indol-5-ylphenylcarbamate tartrate dihydrate (Fenidin D-tartrate Form B), crystalline (3aR)-1, 3a, 8-trimethyl-1, 2, 3, 3a, 8, 8a-hexahydropyrrolo (2, 3-b) indol-5-ylphenylcarbamate tartrate Form A (Fenidin D-tartrate Form A + Pattern C) having peaks of pattern C, and amorphous (3aR)-1, 3a, 8-trimethyl-1, 2, 3, 3a, 8, 8, 8-hexahydropyrrolo (2, 3-b) indol-5-ylphenylcarbamate tartrate Form B) having peaks of pattern C, the invention relates to 1, 3, 5, 7, 8a-hexahydropyrrolo (2, 3-b) indole-5-yl phenyl carbamate tartrate and a preparation method thereof. Also disclosed are pharmaceutical compositions comprising a Fetinil D-tartrate Form A, a Fetinil D-tartrate Form B, a Fetinil D-tartrate Form A having a peak of pattern C, and an amorphous Fetinil D-tartrate, and methods of treating various conditions by administering these solid forms.

The invention relates to a method for separating and detecting olodaterol or salt and enantiomer thereof. The invention provides a method for separating and detecting olodaterol or salts thereof and enantiomers thereof, and belongs to the field of pharmaceutical analysis. According to the separation and detection method, high performance liquid chromatography is adopted, and according to the high performance liquid chromatography, cellulose-tri-(4-chloro-3-methyl phenyl carbamate) or a chromatographic column with cellulose-tri (3, 5-dichlorophenyl carbamate) covalently bonded to the surface of silica gel as a filler is adopted; and a mixed solution of normal hexane, absolute ethyl alcohol and diethylamine is used as a mobile phase. The separation and detection method can quickly separate olodaterol or salts thereof and enantiomers thereof with good separation degree, high sensitivity, high accuracy and good reproducibility.

The invention relates to a fluorescence detection reagent for on-site rapid classification and identification of synthetic cannabinoid. According to the detection reagent, based on a steric hindrance engineering thermodynamic gating strategy, a fluorescent probe molecule tert-butyl (4-(2-(4-hydroxybutyl)-1, 3-dioxo-2, 3-dihydro-1H-benzo [de] isoquinoline-6-yl) phenyl) carbamate containing a specific steric hindrance group (Boc group) is designed and synthesized. And the probe forms a fluorescence quenching aggregate in a thermodynamic metastable state in a system. The aggregate constructs a specific energy threshold value, and only when the aggregate encounters synthetic cannabinoid of a high affinity category (simultaneously having a keto / ester head and a hydrophobic tail chain), dissociation of the aggregate is synergistically triggered through multiple non-covalent interaction, and a remarkable fluorescent lightening signal is generated. The response time is less than 1 s, the detection limit can reach the microgram level, and the method has the characteristics of simplicity and convenience in operation, strong anti-interference performance (no false positive), convenience in visual observation and the like. The problem that a traditional single-molecule probe is difficult to classify and identify synthetic cannabinoid in a complex matrix is solved, and powerful technical support is provided for on-site investigation of drugs.

Solid forms of (3aR)-1, 3a, 8-trimethyl-1, 2, 3, 3a, 8, 8a-hexahydropyrrolo (2, 3-b) indol-5-yl phenyl-carbamate tartrate, including crystalline (3aR)-1, 3a, 8-trimethyl-1, 2, 3, 3a, 8, 8a-hexahydropyrrolo (2, 3-b) indol-5-yl phenyl-carbamate tartrate (posiphen D-tartrate Form A), crystalline (3aR)-1, 3a, 8-trimethyl-1, 2, 3, 3a, 8, 8a-hexahydropyrrolo (2, 3-b) indol-5-yl phenyl-carbamate tartrate dihydrate (posiphen D-tartrate Form B), crystalline (3aR)-1, 3a, 8-trimethyl-1, 2, 3, 3a, 8, 8a-hexahydropyrrolo (2, 3-b) indol-5-yl phenyl-carbamate tartrate Form A having the peak of Pattern C (posiphen D-tartrate Form A+Pattern C), and amorphous (3aR)-1, 3a, 8-trimethyl-1, 2, 3, 3a, 8, 8a-hexahydropyrrolo (2, 3-b) indol-5-yl phenyl-carbamate tartrate, are disclosed. Pharmaceutical compositions comprising posiphen D-tartrate Form A, posiphen D-tartrate Form B, posiphen D-tartrate Form A having the peaks of Pattern C, and amorphous posiphen D-tartrate, and methods of treating various conditions by administering these solid forms, are also disclosed.

The invention relates to a method for detecting enantiomers and diastereoisomers of lumepirone tosylate, which is used for detecting enantiomers and diastereoisomers of lumepirone tosylate by adopting a high performance liquid chromatography. In the high performance liquid chromatography detection process, a filling agent of a chromatographic column is amylose-tri (4-chloro-3-methyl phenyl carbamate), and a mobile phase comprises alkane, alcohol and amine. The detection method has the advantages of good separation degree, high sensitivity and simple method, and is suitable for inspection and quality control of the lumepirone tosylate isomer in the medical industry, so that the safety of clinical medication is improved.

The invention provides a preparation method of silane modified epoxy resin, which comprises the following steps: under the protection of nitrogen, adding 10-50 parts by weight of epoxy resin and 40-60 parts by weight of organosilane containing secondary amine groups into a reaction kettle, heating to 50-60 DEG C under a stirring condition, and reacting for 1-5 hours; adding 10-50 parts by weight of organic silane containing isocyanate functional groups within 1 hour, continuously heating to 70-80 DEG C, and reacting for 1-5 hours; cooling to room temperature and filtering to obtain a target product. By introducing organosilane containing a secondary amine group and organosilane containing an isocyanate functional group, an efficient end-capping reaction of epoxy resin is realized, a modified product of which the molecular structure simultaneously contains an epoxy group, a phenyl group, a carbamate bond and a silane alkoxy group is obtained, the crosslinking sites of the epoxy resin are increased, and the crosslinking property of the epoxy resin is improved. And silane groups acting with a plurality of substrates are introduced, so that the adhesive property on materials such as PC, PET, PBT, PPS, PMMA and PA6 is obviously improved.

The present invention provides a process for chiral resolution of trans-2,2-dichloro-3-(3,5- dichlorophenyl)-cyclopropane-1-carboxylic acid by chiral chromatography using an eluent comprising a mixture of an apolar solvent and a polar co-solvent selected from aliphatic alcohols, ethyl acetate and acetonitrile, and using a chiral stationary phase selected from the list consisting of amylose tris (S)-α-methylbenzyl carbamate, amylose tris (3-chloro-4-methylphenylcarbamate), amylose tris (3,5-dimethylphenylcarbamate) and amylose tris (3-chloro-5-methylphenylcarbamate).

The invention provides a method for detecting an NMV-B00 enantiomer of a nemategravir starting material, and belongs to the field of pharmaceutical analysis. According to the detection method, high performance liquid chromatography is adopted for detection, and an amylose-tri-(4-chlorine-3-methyl phenyl carbamate) chromatographic column, an amylose-tri-((s)-alpha-methyl benzyl carbamate) chromatographic column, a cellulose-tri-(4-methyl benzoate) chromatographic column or a cellulose-tri-(3, 4-dichlorophenyl)-3-(4-chloro-3-methyl phenyl carbamate) chromatographic column is adopted as a chromatographic column. The method comprises the following steps: taking a covalent bond bonded chromatographic column of 2, 5-dichlorophenyl carbamate as a separation chromatographic column, and taking a mixed solution of n-hexane and an alcoholic solution of acid as a mobile phase for elution. The detection method is good in separation degree, high in sensitivity, high in accuracy, good in reproducibility and high in durability.

The invention relates to a chiral separation analysis method of a tefuryltrione enantiomer, and belongs to the field of chiral chromatographic separation and analytical chemistry. Comprising the following steps: 1, diluting raceme tefuryltrione with acetonitrile to prepare a test solution with the concentration of 10mg / L; 2, carrying out enantiomer separation analysis on the raceme tefuryltrione by adopting a reversed-phase high-performance liquid chromatography carried chiral stationary phase; a mobile phase in the liquid chromatography is a binary mobile phase composed of a formic acid aqueous solution and an acetonitrile organic solvent, and the content of formic acid in the formic acid aqueous solution is more than 0 and less than or equal to 1.0%; the chiral stationary phase is polysaccharide derivative bonding type amylose-tri (3-chloro-5-methyl phenyl carbamate). The method has the advantages that the polysaccharide derivative bonded amylose-tri (3-chloro-5-methyl phenyl carbamate) is used as the chiral stationary phase, the separation degree of the tefuryltrione enantiomers is greater than 1.5, and the baseline separation between the enantiomers is successfully realized.

Solid forms of (3aR)-l, 3a, 8-trimethyl-l, 2, 3, 3a, 8, 8a-hexahydropyrrolo (2, 3-b) indol- 5-yl phenyl-carbamate tartrate, including (3aR)-l, 3a, 8-trimethyl-l, 2, 3, 3a, 8, 8a- hexahydropyrrolo (2, 3-b) indol-5-yl phenyl-carbamate tartrate (posiphen D-tartrate Form A), (3aR)-l, 3a, 8-trimethyl-l, 2, 3, 3a, 8, 8a-hexahydropyrrolo (2, 3-b) indol-5-yl phenyl-carbamate tartrate dihydrate (posiphen D-tartrate Form B) and methods of preparing the same are disclosed.