Category: 2525-16-8

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 2525-16-8, name is 7-Methoxy-3,4,5,6-tetrahydro-2H-azepine belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 7-Methoxy-3,4,5,6-tetrahydro-2H-azepine

To a solution of ethyl N-[3-(3-amidinophenyl)-2-(E)-propenyl]-N-[3-chloro-4-(piperidin-4-yloxy)phenyl]sulfamoylacetate dihydrochloride (0.75 g) obtained in example 47(a) in ethanol (25 ml) were added successively 7-methoxy-3,4,5,6-tetrahydro-2H-azepine (0.39 g) and triethylamine (0.85 ml) at room temperature, and the resulting mixture was stirred at room temperature for 7 hours and then allowed to stand at room temperature for 15 hours.. Because of the slow progress of the reaction, 7-methoxy-3,4,5,6-tetrahydro-2H-azepine (0.22 g) and triethylamine (0.51 ml) were furthermore added successively, and the resulting mixture was stirred at 45C for 12 hours, allowed to stand at room temperature for 11 hours and then furthermore stirred at 45C for 10 hours.. After stirring, to the reaction mixture was added a 4N solution of hydrogen chloride in dioxane (5 ml) and the resulting mixture was evaporated in vacuo.. The residue obtained was purified by preparative HPLC (YMC-Pack ODS-A; YMC, eluent: 25 % acetonitrile/water).. Subsequently, to a solution of the amorphous solid obtained in ethanol (5 ml) was added a 4N solution of hydrogen chloride in dioxane (2 ml), and the resulting mixture was evaporated to dryness in vacuo.. The residue obtained was dissolved in water and then lyophilized to afford the title compound (0.30 g, yield: 35 %) as a colorless amorphous solid. 1H NMR (400MHz, DMSO-d6) delta ppm: 1.21 (3H, t, J=7.0), 1.52-1.63 (4H, m), 1.68-1.81 (4H, m), 2.04-2.10 (2H, m), 2.84-2.88 (2H, m), 3.36-3.42 (2H, m), 3.62-3.91 (4H, m), 4.18 (2H, q, J=7.0), 4.41 (2H, s), 4.46 (2H, d, J=6.0), 4.81-4.87 (1H, m), 6.44 (1H, dt, J=16.0, 6.0), 6.57 (1H, d, J=16.0), 7.32 (1H, d, J=9.0), 7.40 (1H, dd, J=9.0, 2.5), 7.52- 7.59 (2H, m), 7.66-7.74 (2H, m), 7.88 (1H, s); IR (KBr, cm-1): 1738, 1674, 1628, 1353, 1156.

The synthetic route of 2525-16-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sankyo Company, Limited; EP1375482; (2004); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 2525-16-8, name is 7-Methoxy-3,4,5,6-tetrahydro-2H-azepine, A new synthetic method of this compound is introduced below., Application In Synthesis of 7-Methoxy-3,4,5,6-tetrahydro-2H-azepine

I. 3-Methyl-7,8,9,10-tetrahydroazepino[2,1-b]quinazolin-12(6H)-one 25 g 2-bromo-4-methylbenzoic acid was treated with 150 mL of 28% aqueous ammonia, 50 g gaseous ammonia, 1 g CuSO4 at 140 C. for 12 hours in an autoclave, then concentrated in vacuo, dissolved in a minimal amount of water, pH adjusted to 6 with 4N HCl. The precipitate was filtered, washed with ice cold water, and dried at 60 C. The residue was extracted with THF and concentrated in vacuo, giving a light brown crystalline solid. Yield of combined material: 14 g 4-methylanthranilic acid. 6.4 g of this acid was suspended with stirring in 100 mL toluene. 11 mL 1-Aza-2-methoxy-1-cycloheptene (1) (Aldrich) were added and the mixture was refluxed under a Dean-Stark trap for 12 hours. Then the toluene was removed by distillation in vacuo, followed by removal of excess (1) in vacuo (11 mm Hg) at 140 C. The dark brown residue crystallized. It was purified by column chromatography (6:1 chloroformethyl acetate) followed by recrystallization from hexane-ethyl acetate to give 7.1 g of pure 3-methyl-7,8,9,10-tetrahydroazepino[2,1-b]quinazolin-12(6H)-one as white, shiny crystals.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Warner-Lambert Company; US5486512; (1996); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Reference of 2525-16-8, These common heterocyclic compound, 2525-16-8, name is 7-Methoxy-3,4,5,6-tetrahydro-2H-azepine, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

To a solution of ethyl N-[3-(3-amidinophenyl)-2-(E)-propenyl]-N-[3-methyl-4-(piperidin-4-yloxy)phenyl]sulfamoylacetate (640 mg) obtained in example 65(a) in ethanol (12 ml) were added successively 7-methoxy-3,4,5,6-tetrahydro-2H-azepine (348 mg) and triethylamine (0.26 ml) at room temperature and the resulting mixture was stirred at room temperature for 2.5 days and then evaporated in vacuo.. The residue obtained was purified by preparative HPLC (YMC-Pack ODS-A; YMC, eluent: 20 % acetonitrile/water).. Subsequently, to a solution of the amorphous solid obtained in ethanol (5 ml) was added a 4N solution of hydrogen chloride in dioxane (0.42 ml), and the resulting mixture was evaporated to dryness in vacuo.. The residue obtained was dissolved in water and then lyophilized to afford the title compound (336 mg, yield: 40 %) as a colorless amorphous solid. 1H NMR (400MHz, DMSO-d6) delta ppm: 1.23 (3H, t, J=7.0), 1.52-1.64 (4H, m), 1.68-1.82 (4H, m), 1.98-2.09 (2H, m), 2.17 (3H, s), 2.87 (2H, m), 3.48 (2H, m), 3.65-3.75 (2H, m), 3.77-3.88 (2H, m), 4.19 (2H, q, J=7.0), 4.33 (2H, s), 4.44 (2H, d, J=6.0), 4.74 (1H, m), 6.44 (1H, dt, J=16.0, 6.0), 6.57 (1H, d, J=16.0), 7.06 (1H, d, J=8.5), 7.25 (1H, dd, J=8.5, 2.5), 7.28 (1H, d, J=2.5), 7.55 (1H, t, J=8.0), 7.69 (1H, d, J=8.0), 7.72 (1H, d, J=8.0), 7.89 (1H, s); IR (KBr, cm-1): 1738, 1675, 1628, 1351, 1157.

Statistics shows that 7-Methoxy-3,4,5,6-tetrahydro-2H-azepine is playing an increasingly important role. we look forward to future research findings about 2525-16-8.

Reference:
Patent; Sankyo Company, Limited; EP1375482; (2004); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 2525-16-8, name is 7-Methoxy-3,4,5,6-tetrahydro-2H-azepine, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C7H13NO

To a solution of ethyl N-[3-(3-amidinophenyl)-2-(E)-propenyl]-N-[4-(piperidin-4-yloxy)phenyl]sulfamoylacetate dihydrochloride (0.51 g) obtained in example 59(a) in ethanol (5 ml) were added successively 7-methoxy-3,4,5,6-tetrahydro-2H-azepine (0.34 g) and triethylamine (0.60 ml) at room temperature, and the resulting mixture was stirred at room temperature for 18 hours and then evaporated in vacuo.. The residue obtained was purified by preparative HPLC (YMC-Pack ODS-A; YMC, eluent: 25 % acetonitrile/water).. Subsequently, to a solution of the amorphous solid obtained in ethanol (5 ml) was added a 4N solution of hydrogen chloride in dioxane (1 ml), and the resulting mixture was evaporated to dryness in vacuo.. The residue obtained was dissolved in water and then lyophilized to afford the title compound (0.14 g, yield: 24 %) as a colorless amorphous solid. 1H NMR (400MHz, DMSO-d6) delta ppm: 1.23 (3H, t, J=7.0), 1.46-1.76 (8H, m), 2.01-2.10 (2H, m), 2.86-2.89 (2H, m), 3.45-3.50 (2H, m), 3.57-3.70 (2H, m), 3.85-3.97 (2H, m), 4.20 (2H, q, J=7.0), 4.34 (2H, s), 4.45 (2H, d, J=6.0), 4.70-4.76 (1H, m), 6.45 (1H, dt, J=16.0, 6.0), 6.55 (1H, d, J=16.0), 7.39 (2H, d, J=9.0), 7.54 (2H, d, J=9.0), 7.54 (1H, t, J=8.0Hz), 7.69-7.73 (2H, m), 7.90 (1H, s); IR (KBr, cm-1): 1737, 1674, 1629, 1351, 1158.

According to the analysis of related databases, 2525-16-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Sankyo Company, Limited; EP1375482; (2004); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem