5 results about "Methyl pentanoate" patented technology

The invention belongs to the technical field of organic synthetic chemistry, and discloses a method for efficiently synthesizing methyl 2-chloro-3-oxovalerate. According to the method, high-selectivity chlorination is performed on a beta-site C-H bond of methyl 3-oxovalerate under a mild condition by taking sodium chloride as a chlorine source and adopting a dual-catalysis system consisting of engineered halogenase and a visible light-sensitive catalyst under visible light irradiation. The engineered halogenase is a HalB triple mutant, and the affinity and regioselectivity of a substrate are remarkably improved; the photosensitive catalyst is a ruthenium bipyridine complex and synergistically drives generation of chlorine free radicals. According to the invention, a brand new biological-photochemical synergistic catalysis platform is constructed by organically combining the substrate recognition capability of the engineered halogenase and an electron transfer mechanism driven by visible light catalysis, so that the contradiction among selectivity, mildness and atomic efficiency of a traditional chlorination method is solved; and the method can be expanded to precise synthesis of other beta-functionalized ketone ester compounds.

This invention relates to a novel method for preparing ruxolitinib phosphate. Methyl 4-(1-(2-cyano-1-cyclopentylethyl)-1H-pyrazol-4-yl)-7H-pyrrolo[2,3-D]pyrimidin-7-yl)terpentanoate (compound X) is deprotected under alkaline conditions, then directly resolved without separation, alkalized to release the free ruxolitinib, and salted to obtain the ruxolitinib phosphate. The obtained ruxolitinib phosphate has an HPLC purity >99.90%, and the ruxolitinib phosphate isomer has a purity >99.50%. The preparation method of this invention has the advantages of simple operation, controllable impurities, low cost, and suitability for industrial production.

The application discloses a method for preparing methyl valerate by butene carbonylation, and belongs to the field of catalytic chemistry. Raw materials containing butene, carbon monoxide and methanol are introduced into a reactor loaded with a solid acid catalyst, and a product containing methyl valerate is obtained through reaction. The application provides a new method for preparing methyl valerate by butene carbonylation with a solid acid catalyst. The method for preparing methyl valerate has the advantages of cheap and easily obtained raw materials, small corrosion of the system, easy separation of the product, less waste discharge, easy engineering of the fixed bed process, and suitability for single large-scale production.

The application discloses a method for preparing methyl tert-butyl ether (MTBE) and / or tert-butyl alcohol (TBA) and belongs to the field of heterogeneous catalytic conversion. The method comprises the following steps: contacting raw material gas containing MTBE and / or TBA, CO and a solid acid catalyst, and reacting to obtain methyl pivalate and / or pivalic acid; the solid acid catalyst comprises an acidic zeolite molecular sieve. The method adopts a molecular sieve catalyst to catalyze the carbonylation of MTBE and TBA under gas-solid phase conditions to generate methyl pivalate and pivalic acid, the selectivity of the products is high, the products are easy to separate from the catalyst, the deactivated catalyst can be regenerated, the process is simple and economical, and a new path for preparing high-value-added chemicals from MTBE and TBA is opened up.

The invention relates to a method for detecting impurities in a process for preparing valproic acid, sodium valproate or magnesium valproate by atom economy reaction, which comprises the following steps of: selecting a gas chromatograph with the model of Agilent 8890, and detecting valproic acid prepared by atom economy reaction and process impurities thereof by gas chromatography; the detection conditions of the gas chromatography are as follows: a chromatographic column is DB-FFAP, and the specification is 0.32 mm * 60 m, 0.5 [mu] m; the carrier gas is nitrogen; the detector is an FID (Flame Ionization Detector); the flow rate is 2ml / min; the sample injection volume is 2 microliters; the temperature of a sample inlet is 220 DEG C; the column temperature is 100 DEG C; in the heating procedure, the initial temperature is 100 DEG C and kept for 5 min, then the temperature is increased to 140 DEG C at the speed of 4 DEG C / min and kept for 5 min, and then the temperature is increased to 200 DEG C at the speed of 4 DEG C / min and kept for 15 min; the operation time is 50 min; the temperature of a detector is 220 DEG C; the method comprises the following steps of: injecting 2 microliters of diluent dichloromethane, 2 microliters of reference solution and 2 microliters of test solution into a gas chromatograph, and recording a chromatogram; a test article is selected from a valproic acid crude product prepared by atom economy reaction; the impurities are selected from 2-propyl-4-pentenoic acid, valeric acid, 2-methyl valeric acid, 2-ethyl valeric acid, methyl valproate, ethyl valproate or propyl valproate; the solvent is a solvent; according to the detection result of the gas chromatography, the variety and the content of the process impurities in the valproic acid, the sodium valproate or the magnesium valproate are judged through a control sample.