Patent classifications
C07C253/34
SOLIDIFICATION OR CRYSTALLISATION METHOD
A solidification or crystallization method is disclosed, which includes providing at least a first organic compound and at least one volatile co-former organic compound. A mixture of at least the first organic compound and the co-former organic compound is formed, wherein either the first organic compound or the volatile co-former organic compound includes a hydrogen acceptor moiety and the other includes a hydrogen donor moiety, thereby allowing the formation of hydrogen bonds between the first organic compound and the volatile co-former organic compound. The mixture is allowed to stand for sufficient time for the mixture to liquify at a temperature below that of the melting points of the components, thereby forming a liquid mixture. The volatile co-former organic compound is allowed to evaporate, thereby resulting in crystallization of at least the first organic compound. The method can be a co-crystallization method if there are two organic compounds.
SOLIDIFICATION OR CRYSTALLISATION METHOD
A solidification or crystallization method is disclosed, which includes providing at least a first organic compound and at least one volatile co-former organic compound. A mixture of at least the first organic compound and the co-former organic compound is formed, wherein either the first organic compound or the volatile co-former organic compound includes a hydrogen acceptor moiety and the other includes a hydrogen donor moiety, thereby allowing the formation of hydrogen bonds between the first organic compound and the volatile co-former organic compound. The mixture is allowed to stand for sufficient time for the mixture to liquify at a temperature below that of the melting points of the components, thereby forming a liquid mixture. The volatile co-former organic compound is allowed to evaporate, thereby resulting in crystallization of at least the first organic compound. The method can be a co-crystallization method if there are two organic compounds.
ACETONITRILE PURIFICATION PROCESS FOR ULTRAHIGH PERFORMANCE LIQUID CHROMATOGRAPHY-MASS SPECTROMETER
The present invention relates to the technical field of acetonitrile refining, and in particular, to an acetonitrile purification process for an ultrahigh performance liquid chromatography-mass spectrometer. According to the acetonitrile purification process provided by the present invention, the production cost may be reduced and the yield may be increased to reach 95% or more while the quality of the chromatographic pure acetonitrile is further improved to reach the UPLC-MS level; and an industrial UPLC-MS level acetonitrile purification and preparation method provided by the present invention has the advantages of simple operation, low cost, safety, high efficiency and capability of realizing large-scale industrial production.
ACETONITRILE PURIFICATION PROCESS FOR ULTRAHIGH PERFORMANCE LIQUID CHROMATOGRAPHY-MASS SPECTROMETER
The present invention relates to the technical field of acetonitrile refining, and in particular, to an acetonitrile purification process for an ultrahigh performance liquid chromatography-mass spectrometer. According to the acetonitrile purification process provided by the present invention, the production cost may be reduced and the yield may be increased to reach 95% or more while the quality of the chromatographic pure acetonitrile is further improved to reach the UPLC-MS level; and an industrial UPLC-MS level acetonitrile purification and preparation method provided by the present invention has the advantages of simple operation, low cost, safety, high efficiency and capability of realizing large-scale industrial production.
CIS-PARA-SUBSTITUTED CYCLOHEXYLAMINONITRILE SALT, PREPARATION METHOD THEREFOR AND USE THEREOF, AND METHOD FOR PREPARING PESTICIDE USING SAME
The present application relates to a cis-para-substituted cyclohexylaminonitrile salt represented by formula (I), a preparation method therefor and use thereof as an intermediate for preparing a pesticide, and a method for preparing the pesticide by using same as an intermediate. In the formula, R is C.sub.1-10 alkyl or C.sub.1-10alkyloxy, C.sub.2-10 alkenyl or C.sub.2-10 alkenyloxy, C.sub.2-10 alkynyl or C.sub.2-10 alkynyloxy, C.sub.3-10 cycloalkyl or C.sub.3-10 cycloalkyloxy, C.sub.3-10 heterocycloalkyl or C.sub.3-10 heterocycloalkyloxy containing 1-2 heteroatoms selected from O and N.
##STR00001##
CIS-PARA-SUBSTITUTED CYCLOHEXYLAMINONITRILE SALT, PREPARATION METHOD THEREFOR AND USE THEREOF, AND METHOD FOR PREPARING PESTICIDE USING SAME
The present application relates to a cis-para-substituted cyclohexylaminonitrile salt represented by formula (I), a preparation method therefor and use thereof as an intermediate for preparing a pesticide, and a method for preparing the pesticide by using same as an intermediate. In the formula, R is C.sub.1-10 alkyl or C.sub.1-10alkyloxy, C.sub.2-10 alkenyl or C.sub.2-10 alkenyloxy, C.sub.2-10 alkynyl or C.sub.2-10 alkynyloxy, C.sub.3-10 cycloalkyl or C.sub.3-10 cycloalkyloxy, C.sub.3-10 heterocycloalkyl or C.sub.3-10 heterocycloalkyloxy containing 1-2 heteroatoms selected from O and N.
##STR00001##
HIGH PURITY 2-NAPHTHYLACETONITRILE AND METHOD FOR PRODUCING SAME
High purity 2-naphthylacetonitrile with fewer impurities can be used as a starting material or intermediate for synthesizing various pharmaceutical products, agricultural chemicals, and chemical products, and a production method thereof. A high purity 2-naphthylacetonitrile having an HPLC purity of 2-naphthylacetonitrile of not less than 95 area %, and containing naphthalene compounds represented by the formulas (a)-(j) at a content of a predetermined area % or below. A method for producing high purity 2-naphthylacetonitrile, may include: subjecting 2′-acetonaphthone to a Willgerodt reaction in the presence of an additive where necessary, and hydrolyzing the obtained amide compound to give 2-naphthylacetic acid; and reacting the 2-naphthylacetic acid obtained in the subjecting, a halogenating agent and sulfamide in the presence of a catalyst as necessary in an organic solvent to give 2-naphthylacetonitrile.
HIGH PURITY 2-NAPHTHYLACETONITRILE AND METHOD FOR PRODUCING SAME
High purity 2-naphthylacetonitrile with fewer impurities can be used as a starting material or intermediate for synthesizing various pharmaceutical products, agricultural chemicals, and chemical products, and a production method thereof. A high purity 2-naphthylacetonitrile having an HPLC purity of 2-naphthylacetonitrile of not less than 95 area %, and containing naphthalene compounds represented by the formulas (a)-(j) at a content of a predetermined area % or below. A method for producing high purity 2-naphthylacetonitrile, may include: subjecting 2′-acetonaphthone to a Willgerodt reaction in the presence of an additive where necessary, and hydrolyzing the obtained amide compound to give 2-naphthylacetic acid; and reacting the 2-naphthylacetic acid obtained in the subjecting, a halogenating agent and sulfamide in the presence of a catalyst as necessary in an organic solvent to give 2-naphthylacetonitrile.
Tricyanohexane purification methods
Provided herein are processes for purifying TCH in a feed stream, such as an adiponitrile process stream. The processes include a first separating step of separating the adiponitrile process stream to form a first overhead stream comprising low-boiling components and high-boiling components and a first bottoms stream comprising high-boiling components. The processes also include a second separating step of separating the first overhead stream in one or more distillation columns to form a lights stream comprising low-boiling components, a heavies stream comprising high-boiling components, and a TCH stream.
Tricyanohexane purification methods
Provided herein are processes for purifying TCH in a feed stream, such as an adiponitrile process stream. The processes include a first separating step of separating the adiponitrile process stream to form a first overhead stream comprising low-boiling components and high-boiling components and a first bottoms stream comprising high-boiling components. The processes also include a second separating step of separating the first overhead stream in one or more distillation columns to form a lights stream comprising low-boiling components, a heavies stream comprising high-boiling components, and a TCH stream.