A synthetic method of 9,9-bis[4-(2-hydroxyethoxy)phenyl]fluorene, belonging to the technical field of chemical synthesis. 9-fluorenone, phenoxyethanol, a catalyst and a cocatalyst are stiffed in an alkane solvent and heated until refluxing, the generated water is removed from the reaction solution via an azeotropic method while reacting, the reaction solution is diluted with water after the reaction is ended, uniformly stirred and cooled to separate out crystals and then filtered, a filter cake is rinsed and dried to obtain a 9,9-bis[4-(2-hydroxyethoxy)phenyl]fluorene finished product; the filtered crystallization mother liquor is subjected to standing and layering, a water phase is removed, then an organic phase is distilled to recycle the alkane solvent, and the concentrate is rectified to recycle phenoxyethanol.

A synthetic method of 9,9-bis[4-(2-hydroxyethoxy)phenyl]fluorene, belonging to the technical field of chemical synthesis. 9-fluorenone, phenoxyethanol, a catalyst and a cocatalyst are stiffed in an alkane solvent and heated until refluxing, the generated water is removed from the reaction solution via an azeotropic method while reacting, the reaction solution is diluted with water after the reaction is ended, uniformly stirred and cooled to separate out crystals and then filtered, a filter cake is rinsed and dried to obtain a 9,9-bis[4-(2-hydroxyethoxy)phenyl]fluorene finished product; the filtered crystallization mother liquor is subjected to standing and layering, a water phase is removed, then an organic phase is distilled to recycle the alkane solvent, and the concentrate is rectified to recycle phenoxyethanol.

Provided is a production method capable of efficiently producing a reduced coenzyme Q10 Form II crystal. A method for producing reduced coenzyme Q10 crystals comprises warming a mixture of a reduced coenzyme Q10 Form I crystal and a reduced coenzyme Q10 Form II crystal to 32° C. or higher, in the presence of 0.001 to 50 parts by weight of a solvent with respect to 100 parts by total weight of the crystals, so as to increase the content of the reduced coenzyme Q10 Form II crystal. The warming time may be 1 hour or more and less than 14 hours, and after the warming of the mixture in the presence of the solvent, drying may be performed at 45° C. or higher to remove the solvent.

Provided is a production method capable of efficiently producing a reduced coenzyme Q10 Form II crystal. A method for producing reduced coenzyme Q10 crystals comprises warming a mixture of a reduced coenzyme Q10 Form I crystal and a reduced coenzyme Q10 Form II crystal to 32° C. or higher, in the presence of 0.001 to 50 parts by weight of a solvent with respect to 100 parts by total weight of the crystals, so as to increase the content of the reduced coenzyme Q10 Form II crystal. The warming time may be 1 hour or more and less than 14 hours, and after the warming of the mixture in the presence of the solvent, drying may be performed at 45° C. or higher to remove the solvent.

The present generally relates to an improved process for the preparation of dapagliflozin of Formula I or its solvates or co-crystals thereof. The present invention also encompasses the novel intermediates and their use in the preparation of dapagliflozin.

The present generally relates to an improved process for the preparation of dapagliflozin of Formula I or its solvates or co-crystals thereof. The present invention also encompasses the novel intermediates and their use in the preparation of dapagliflozin.

The present invention relates to a stable crystal form, i.e. form A, of 2-tert-butyl-4-methoxyphenol, and to a new preparation method for the 2-tert-butyl-4-methoxyphenol; and the use of the 2-tert-butyl-4-methoxyphenol and the stable crystal form thereof, i.e. form A, in preparing antitumor drugs or immunomodulator drugs. The stable crystal form, i.e. form A, as expressed by a powder X-ray diffraction pattern in an angle of 2θ, using Cu-Kα radiation, has at least 3 absorption peaks selected from the following positions: 6.27±0.10, 6.94±0.10, 12.27±0.10, 13.36±0.10, 14.01±0.10, 14.79±0.10, 15.31±0.10, 17.05±0.10, 18.30±0.10, 19.00±0.10, 20.47±0.10, 20.98±0.10, 22.37±0.10, 23.68±0.10, 24.55±0.10, 25.37±0.10, 30.83±0.10, 33.12±0.10, 40.50±0.10, 42.81±0.10.

The present invention relates to a stable crystal form, i.e. form A, of 2-tert-butyl-4-methoxyphenol, and to a new preparation method for the 2-tert-butyl-4-methoxyphenol; and the use of the 2-tert-butyl-4-methoxyphenol and the stable crystal form thereof, i.e. form A, in preparing antitumor drugs or immunomodulator drugs. The stable crystal form, i.e. form A, as expressed by a powder X-ray diffraction pattern in an angle of 2θ, using Cu-Kα radiation, has at least 3 absorption peaks selected from the following positions: 6.27±0.10, 6.94±0.10, 12.27±0.10, 13.36±0.10, 14.01±0.10, 14.79±0.10, 15.31±0.10, 17.05±0.10, 18.30±0.10, 19.00±0.10, 20.47±0.10, 20.98±0.10, 22.37±0.10, 23.68±0.10, 24.55±0.10, 25.37±0.10, 30.83±0.10, 33.12±0.10, 40.50±0.10, 42.81±0.10.

Provided is a production method capable of efficiently producing a reduced coenzyme Q10 Form II crystal. The method for producing a reduced coenzyme Q10 Form II crystal includes: adding a reduced coenzyme Q10 Form II crystal as a seed crystal to a solution with a temperature of 32° C. to 43° C., the solution containing fa) at least one organic solvent selected from the group consisting of an alcohol, a hydrocarbon, an aliphatic acid ester and a nitrogen compound, and (b) reduced coenzyme Q10, to prepare a mixture, and precipitating the reduced coenzyme Q10 from the mixture, in the form of the reduced coenzyme Q10 Form II crystal.

Provided is a production method capable of efficiently producing a reduced coenzyme Q10 Form II crystal. The method for producing a reduced coenzyme Q10 Form II crystal includes: adding a reduced coenzyme Q10 Form II crystal as a seed crystal to a solution with a temperature of 32° C. to 43° C., the solution containing fa) at least one organic solvent selected from the group consisting of an alcohol, a hydrocarbon, an aliphatic acid ester and a nitrogen compound, and (b) reduced coenzyme Q10, to prepare a mixture, and precipitating the reduced coenzyme Q10 from the mixture, in the form of the reduced coenzyme Q10 Form II crystal.