68results about How to "High isolation yield" patented technology

To provide: a production method using a catalyst which can substantially suppress leaching of active metal components and exhibit high activity for both reactions of transesterification of glycerides and esterification of free fatty acids each contained in a fat or oil; and the catalyst. A method for producing fatty acid alkyl esters and/or glycerin comprising a step of bringing a fat or oil into contact with an alcohol in the presence of a catalyst, wherein the catalyst is at least one catalyst selected from the group consisting of the following (I) to (V):

• • (I) a metal oxide having an ilmenite structure and/or a slyrankite structure;
  • (II) an oxide containing a metallic element belonging to the Group 12 and a metallic element belonging to the Group 4;
  • (III) a mixed oxide containing a metallic element belonging to the Group 12 and a tetravalent transition metallic element;
  • (IV) a metal oxide containing zirconium and at least one metallic element selected from the group consisting of metallic elements belonging to the Groups 4, 5 and 8; and
  • (V) a metal oxide containing anatase type titanium oxide and/or rutile type titanium oxide, and the metal oxide containing a sulfur component of 700 ppm or less.

The invention relates to a novel process for the preparation of dronedarone (I) and pharmaceutically acceptable salts thereof which comprises oxidizing a compound of formula (IV) or a salt thereof with an oxidizing agent in an organic or inorganic solvent or solvent mixture, and isolating the obtained product and, if desired, converting it into a pharmaceutically acceptable salt thereof. Further aspects of the invention include the novel intermediary compound of formula (IV), and a process for the preparation thereof.

A method for synthesizing a deuterated acrylate of the Formula (1), the method comprising: (i) deuterating a propiolate compound of Formula (2) to a methyne-deuterated propiolate compound of Formula (3) in the presence of a base and D₂O: and (ii) reductively deuterating the methyne-deuterated propiolate compound of Formula (3) in a reaction solvent in the presence of deuterium gas and a palladium-containing catalyst to afford the deuterated acrylate of the Formula (1). The resulting deuterated acrylate compounds, derivatives thereof, and polymers derived therefrom are also described.

The invention relates to the pharmaceutical technical field. The extraction method of apigenin comprises the steps of 1) enzymatically hydrolyzing celery which is taken as a substrate for 10 hours at 30-35 DEG C through a mixing solution of apigenin which is 33-37% and glucosidase which is 43-47% in mass percentage concentration; and 2) ultrasonically extracting enzymatic hydrolysate obtained from the step 1) through an ethanol solution of 70%, condensing an extracting solution, extracting respectively through petroleum ether and ethyl acetate, evaporating the extracting solution, dissolving through ethanol of 70%, and separating and extracting through a high performance liquid chromatograph. The pharmaceutical composition for treating diabetes consists of apigenin and glucobay at mass ratio of 1: (2-5). The extraction method, which extracts apigenin through a multi-enzymatic process, greatly improves extraction yield. The pharmaceutical composition disclosed by the invention not only can effectively control blood sugar but also can avoid circumstances of low blood sugar and rapid weight loss of a patient due to simple use of a diabetes medicine.

Disclosed herein is a cost effective and industrially feasible process for the preparation of (+) Clopidogrel bisulphate. The present invention further discloses a novel method of precipitation of (+) Clopidogrel bisulphate Form I directly from solvent mix of methanol and acetone in presence of sulfuric acid at a temperature of 25-40° C.

The invention relates to a novel process for the preparation of dronedarone (I) and pharmaceutically acceptable salts thereof (formula I), which comprises oxidizing a compound of formula (VI), or a salt thereof and the obtained product is isolated and, if desired, converted into a pharmaceutically acceptable salt thereof. Further aspects of the invention include the novel intermediary compound of formula (VI) and process for the preparation thereof.

The invention discloses a synthesis method of an aromatic vinyl trifluoromethylthio ether compound, and belongs to the technical field of chemical synthesis. According to the synthesis method disclosed by the invention, the aromatic vinyl trifluoromethylthio ether compound is prepared by taking trans-nitro aryl ethylene as a substrate, silver trifluoromethylthio as a thioether reagent and copper trifluoroacetic acid as a catalyst, and adding an oxidizing agent and an additive. Raw materials used by the method are easy to obtain, the reaction is simple to operate, the yield is high, and the substrate universality is good; the obtained aromatic vinyl trifluoromethylthio ether product has important application in the medicine, pesticide and function material fields.

The invention provides silica hybrid dehydroherbac, namely, 1-(3-silica hybrid-3, 3-dimethyl cyclohexyl-1-alkenyl) butanone. The silica hybrid dehydroherbac is shown in the formula I. The compound is a perfume compound with strong herb fragrance and oriental arborvitae fragrance and is also an important precursor of an organosilicon perfume compound corresponding to the perfume compounds including herbac, Roman musk, helvetolide and the like. Under the action of palladium catalysis, an inserting ring expansion reaction is conducted on silacyclobutane by end group alkyne, and the silica hybrid dehydroherbac is prepared with high yield. According to a method for preparing the silica hybrid dehydroherbac, raw materials are easy to obtain, the application range is wide, the separation production rate is high, experiment devices are simple, operation is easy to conduct, and industrialization is facilitated.

The invention provides a 1, 3-thiazole derivative and a synthesis method thereof. A 2-acylamino thiazole derivative is prepared from carbodiimide, acyl chloride, a terminal alkyne compound and elemental sulfur. The yield is higher, and the synthesis method is scientific and reasonable, so that a universal method for synthesizing the 2-acylamino thiazole derivative with various substituent groups is provided. The method has the advantages that the raw materials are easily available, and the application range is large, the separating rate is high, experimental devices and operations are simple and easy to operate; therefore, the 1, 3-thiazole derivative can be further developed and used.

The invention belongs to the field of photochemical organic synthesis, and particularly relates to a photochemical synthesis method of an imidazolidine compound. The photochemical synthesis method comprises the step that alcohol reacts with imine in the presence of light and a photocatalyst to obtain the imidazolidine compound. According to the photochemical synthesis method of the imidazolidine compound, the alcohol and imine dissolved in an inert organic solvent are utilized to realize the reaction of synthesis of the imidazolidine compound from the green low-toxic alcohol and imine by controlling the reaction time under the action of the photocatalyst under the induction of ultraviolet light or visible light, and the imidazolidine compound can be obtained. Moreover, the product of the photochemical synthesis method has high yield and good selectivity. The separation yield of the product is up to more than 95% and the selectivity is up to more than 99%. In addition, a preparation process is simple, the product can be obtained by one-step reaction, and the photochemical synthesis method is economical and environmentally friendly, and convenient to operate, and has high practicability.

The invention provides a carbohydrate alkyl bonding imidazole type N-heterocyclic carbene palladium coordination compound as well as a preparation method and application thereof. A structure of the carbohydrate alkyl bonding imidazole type N-heterocyclic carbene palladium coordination compound is shown in a formula I: the formula (1) is shown in the description, wherein R is alkyl, benzyl or aryl,and n is equal to 2 to 10. According to the carbohydrate alkyl bonding imidazole type N-heterocyclic carbene palladium coordination compound disclosed by the invention, by using natural chiral compound D-glucose with low cost, easy availability, good water solubility and rich stereochemistry as a chiral source of the carbohydrate alkyl bonding imidazole type N-heterocyclic carbene palladium coordination compound, under a condition of no additional addition of an alkaline additive, a carbohydrate alkyl bonding imidazole type N-heterocyclic carbene palladium complex I is synthesized by adoptinga quick one-step method and is used as a palladium catalyst for catalyzing C-C coupled reaction, and no-water no-oxygen reaction conditions are overcome, so that a series of fluorene-derived conjugated small molecular functional materials having novel structures are prepared in a high yield manner.

The invention discloses a preparation method for 6-carboxylfluorescein. The method comprises the following steps: a. reacting; b. crystallizing; and c. hydrolyzing. The preparation method prepares 6-carboxylfluorescein by using a metal catalyst of stannic chloride (SnCl4) to selectively catalyze the reaction, and selects an appropriate solvent mixing ratio and an appropriate purification method. Compared with the prior art, the ratio of the required product 6-carboxylfluorescein and the by-product 5-carboxylfluorescein is improved from 1:1 to 2.6:1, and the separation yield is improved from 32% to 61% (1.9 times as much as the past). The method greatly reduces the production cost, simplifies the purification process, provides a practical and efficient novel process method for the preparation of 6-carboxyfluorescein and derivatives thereof which are widely used for fluorescence labeling of biological macromolecules, and has a high application value.

The invention discloses a synthesis method of an aryl thiophthene derivative, which belongs to the field of organic synthesis. The method comprises the following steps of: a) mixing and reacting a compound shown as a formula I and a compound shown as a formula II in an ether solvent, wherein a reaction temperature is between the freezing point of the solvent and room temperature; b) adding zinc powder, raising the reaction temperature to be between 110 DEG C and the boiling point of the solvent and reacting so as to obtain the aryl thiophthene derivative shown as a formula III, wherein R1 and R2 independently represent substituted or unsubstituted alkyl with 1 to 18 carbon atoms, naphthenic base with 3 to 6 carbon atoms, aryl with 6 to 12 carbon atoms or heterocyclic aryl with 2 to 12 carbon atoms; Ar represents aryl with 6 to 12 carbon atoms or heterocyclic aryl with 2 to 12 carbon atoms; and X represents halogen. The synthesis method can be applied to organic photoelectric materials and relevant fields.

The invention discloses a method for synthesizing a quinolin-2-imide derivative. According to the method, the quinolin-2-imide derivative is prepared by using diaryl iodonium ions, carbodiimide, alkyne and a copper catalyst, the yield is relatively high, the synthesis method is scientific and reasonable, and thus, a universal method for synthesizing the quinolin-2-imide derivative with a variety of substituents by a three-component-reaction one-pot process is provided. According to the method, the raw materials are cheap and readily available, the catalyst is cheap, the applicable range is wide, the yield of separation is high, the regioselectivity is good, and the experimental facilities and operation are easy and feasible, so that further development and application are facilitated.

The invention provides a process for the preparation of a compound of the formula:

or an acid addition or base salt thereof, wherein R is phenyl optionally substituted by 1 to 3 substituents each independently selected from halo and trifluoromethyl;

• R¹ is C₁-C₆ alkyl; and
• “Het” is pyrimidinyl optionally substituted by 1 to 3 substituents each independently selected from C₁-C₄ alkyl, C₁-C₄ alkoxy, halo, oxo, benzyl and benzyloxy,

comprising reaction of a compound of the formula:

wherein R is as previously defined for a compound of the formula (I), with a compound of the formula:

wherein R¹ and “Het” are as previously defined for a compound of the formula (I) and X is chloro, bromo or iodo, in the presence of zinc, iodine and/or a Lewis acid and an aprotic organic solvent: said process being optionally followed by conversion of the compound of the formula (I) to an acid addition or base salt thereof.

The invention belongs to the technical field of organic synthesis, and particularly relates to a method for separating formic acid and levulinic acid from hydrate molten salt. The method comprises the following steps: reacting under the coexistence of levulinic acid, formic acid and alcohol in hydrate molten salt, respectively reacting formic acid and levulinic acid with alcohol to generate formate and levulinic acid ester, and carrying out ester exchange on formate and levulinic acid to generate levulinic acid ester and formic acid, after the reaction is finished, the reaction liquid contains levulinic acid ester, formate, levulinic acid, formic acid and alcohol, separating the reaction liquid to obtain an organic phase, distilling the organic phase to respectively obtain levulinic acid ester and formate, and hydrolyzing to respectively obtain levulinic acid and formic acid. The method is simple in technological process, low in energy consumption and easy to separate, and the product can be spontaneously separated from the hydrate molten salt, so that the subsequent purification cost is reduced.