Category: 38041-19-9

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.38041-19-9,Tetrahydro-2H-pyran-4-amine,as a common compound, the synthetic route is as follows.

To a flask having an inner volume of 100 ml, made of glass and equipped with a stirring device, a thermometer and a reflux condenser were charged 30.0 g (158.7 mmol) of 4-hydrazinotetrahydropyran hydrochloride with a purity of 99percent and synthesized in the same manner as in Example 2(1), 3.0 g (0.70 mmol calculated as palladium atom) of 5percent by weight palladium/carbon (50percent wet product) and 150 ml of ethanol, and the mixture was reacted at 75¡ãC for 24 hours under hydrogen atmosphere (0.1 MPa. After completion of the reaction, the reaction mixture was cooled to room temperature and filtered, and the filtrate was concentrated under reduced pressure. When the concentrate was analyzed (internal standard method) by gas chromatography, 15.9 g (Reaction yield: 72percent) of 4-aminotetrahydropyran was found to be formed. Then, 200 ml of n-butyl alcohol and 17.4 g (166.8 mmol) of 12 mol/l hydrochloric acid were added to the concentrate, and the mixture was concentrated under reduced pressure to obtain 14.3 g (Isolation yield: 65percent) of 4-aminotetrahydropyran hydrochloride with a purity of 98percent (areal percentage by gas chromatography) as white crystals. Physical properties of the 4-aminotetrahydropyran hydrochloride were the same as those in Example 2(2).; To a flask having an inner volume of 100 ml, made of glass and equipped with a stirring device, a thermometer and a reflux condenser were charged 1.0 g (5.55 mmol) of 4-hydrazinotetrahydropyran hydrochloride with a purity of 99percent and synthesized in the same manner as in Example 2(1), 6.2 ml of ethanol, 1.2 ml (1.20 mmol) of 1 mol/l aqueous sodium hydroxide solution and 1.5 g (10 mmol) of copper (I) oxide, and the mixture was reacted at 65¡ãC for 1 hour. After completion of the reaction, the reaction mixture was cooled to room temperature and filtered, and the filtrate was concentrated under reduced pressure. When the concentrate was analyzed (internal standard method) by gas chromatography, 0.47 g (Reaction yield: 50percent) of 4-aminotetrahydropyran was found to be formed. Then, 5 ml of n-butyl alcohol and 10 ml (12.0 mmol) of 12 mol/l hydrochloric acid were added to the concentrate, and the resulting mixture was concentrated under reduced pressure to obtain 0.42 g (Isolation yield: 45percent) of 4-aminotetrahydropyran hydrochloride with a purity of 98percent (areal percentage by gas chromatography) as white crystals. Physical properties of the 4-aminotetrahydropyran hydrochloride were the same as those in Example 2(2)., 38041-19-9

The synthetic route of 38041-19-9 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Ube Industries, Ltd.; EP1661894; (2006); A1;,
Tetrahydropyran – Wikipedia
Tetrahydropyran – an overview | ScienceDirect Topics

38041-19-9, Tetrahydro-2H-pyran-4-amine is a Tetrahydropyrans compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a flask having an inner volume of 20 L, made of glass and equipped with a stirring device, a thermometer, a dropping funnel and a reflux condenser were charged 5873 g (115 mol) of 98percent aqueous hydrazine solution and 2072 ml of ethanol, and the mixture was heated to 75¡ãC with stirring. Then, a solution in which 2136 g (11.5 mol) of tetrahydropyranyl-4-methanesulfonate with a purity of 70percent had been dissolved in 2072 ml of ethanol was gradually added dropwise to the mixture, and the mixture was reacted at the same temperature for 4 hours with stirring. After completion of the reaction, the mixture was cooled to room temperature to obtain a reaction mixture comprising 4-hydrazinotetrahydropyran as a main product. Then, to a flask having an inner volume of 20 L, made of glass and equipped with a stirring device, a thermometer, a dropping funnel and a reflux condenser were charged 414.4 g (4.6 mol calculated as nickel atom) of 65percent by weight developed Raney nickel and 2072 ml of water, and the mixture was heated up to 60¡ãC with stirring. Then, the reaction mixture was gradually added dropwise, and the resulting mixture was reacted at 80¡ãC for 2 hours with stirring. After completion of the reaction, the reaction mixture was cooled up to 40¡ãC, Raney nickel was filtered off, and the filtrate was concentrated under reduced pressure to obtain 818.0 g of the reaction solution containing 4-aminotetrahydropyran as a main product. To a flask having an inner volume of 20 L, made of glass and equipped with a stirring device, a thermometer, a dropping funnel, a reflux condenser and a distillation device under reduced pressure were charged the above reaction solution, 2072 ml (10.9 mol) of tetraethylenepentamine and 4100 ml of n-butyl alcohol, and the mixture was stirred at 80¡ãC for 2 hours under reduced pressure. Then, 4-aminotetrahydropyran and n-butyl alcohol were removed by azeotropic distillation under reduced pressure. Thereafter, 4100 ml of n-butyl alcohol was added again, 4-aminotetrahydropyran and n-butyl alcohol were removed by azeotropic distillation under reduced pressure. This operation was repeated to three times to obtain 15000 ml of a distilled solution in total. To the distilled solution was added 575 ml (6.90 mol) of conc. hydrochloric acid, and then, the mixture was concentrated under reduced pressure. To the concentrate was again added 8200 ml of n-butyl alcohol, and water and n-butyl alcohol were removed by azeotropic distillation under reduced pressure. Then, 7460 ml of n-butyl alcohol and 3730 ml of ethanol were added to the residue, and the resulting mixture was once heated up to 115¡ãC and stirred, then, it was gradually cooled to -5¡ãC and stirred for 30 minutes. After the filtration, the filtrate was washed with cooled toluene and dried to obtain 788.9 g (Isolation yield based on tetrahydropyranyl-4-methanesulfonate: 50percent) of 4-aminotetrahydropyran hydrochloride with a purity of 99percent (internal standard method by gas chromatography) as white needle-like crystals. Physical properties of the 4-aminotetrahydropyran hydrochloride were the same as those in Example 2(2).

38041-19-9 Tetrahydro-2H-pyran-4-amine 419223, aTetrahydropyrans compound, is more and more widely used in various.

Reference£º
Patent; Ube Industries, Ltd.; EP1661894; (2006); A1;,
Tetrahydropyran – Wikipedia
Tetrahydropyran – an overview | ScienceDirect Topics