Category: 148870-57-9

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. 148870-57-9, name is 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one, A new synthetic method of this compound is introduced below., Recommanded Product: 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one

A mixture of (S)-N- [(4,5 -dimethoxybenzocyclobut- 1 -yl)methyl] -N-(methyl)amine hydrochloride (lOOg) and d.imethyl formamide (400mL) was stirred for about 5mm and potassium carbonate (178.46g) was added to it. The reaction mixture was stirred forabout lh at about room temperature. The reaction mixture was cooled to about 5C to about 10C. 7, 8-dimethoxy-3 -[3 -iodopropyl] – 1,3 -dihydro-2H-3 -benzazepin-2-one (3 6g) prepared as in Example 8, was added to the stirred reaction mixture. The reaction mixture was stirred for about 4h at about 20C to about 25C. The reaction mixture was quenched into chiHed demineralized water at about 5C to about 10C. The reaction mixture wasacidified to pH of about I to about 2 using concentrated hydrochloric acid and ethyl acetate was added to it. The reaction mixture was stirred and the two layers were separated. The aqueous layer was basified to pH of about 8 to about 9.5 using 20-25% aqueous ammonia solution and ethyl acetate was added to it. The reaction mixture was stirred and the two layers were separated. The organic layer was washed withdemineralized water and concentrated under reduce pressure at about below 55C.Yield: 75%; HPLC purity: > 96%

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; GLENMARK PHARMACEUTICALS LIMITED; GLENMARK GENERICS LIMITED; BHIRUD, Shekhar Bhaskar; BHUSHAN, Kumar Hari; ZOPE, Sunil Sudhakar; PATIL, Dipak Vinayak; DHEBADE, Pramod Amrutrao; CHAND, Prem; WO2014/102827; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

148870-57-9, name is 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Safety of 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one

Example 3: Preparation of 3-{3-[(3,4-dimethoxy-bicyclo[4.2.0]octa-l,3,5-trien-7- ylmethyl)-methyl-amino]-propyl}-7,8-dimethoxy-l,3-dihydro-benzo[d]azepin-2- one (Formula-6) 7,8-Dimethoxy-3-(3-iodopropyl)- 1 ,3-dihydro-2H-3-benzazepin-2-one (Formula-4) (17.8g, 0.0456mol.) is added with (lS)-4,5-Dimethoxy-l-[(methylamino)methyl] benzocyclobutane hydrochloride (Formula-5) (9.29g, 0.0381mol.) in about 107ml. Acetone. To the mass, Potassium carbonate (12.7g, 0.0919mol.) is added and stirred for about 3hr. at 55 – 58C. The mass is filtered through celite bed at 35 – 40C. Filtrate is concentrated under reduced pressure at 45 – 50C to 1.4w/w. To the residual mass, 89ml of ethyl acetate is added and the product is extracted using 3N HC1 solution thrice (89ml, 2 x 35.6ml). The combined aqueous layer is basified using Sodium hydroxide and extracted the product using ethyl acetate thrice (89ml. 2 x 36.5ml). The combined organic layer is washed with water and then concentrated under vacuum at 45 – 50C to obtain about 19.29g (85%) of 3-{3-[(3,4-dimethoxy-bicyclo[4.2.0]octa-l,3,5-trien-7-ylmethyl)- methyl-amino]-propyl}-7,8-dimethoxy-l,3-dihydro-benzo[d]azepin-2-one (Formula-6) having the purity >75%>

The synthetic route of 148870-57-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BIOCON LIMITED; KOTHAKONDA, Kiran Kumar; RAMASAMY, Sivakumar; BANDARU, Sravan Kumar; VENKATA, Srinivas Pullela; WO2014/20534; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 148870-57-9, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 148870-57-9 name is 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Example 6 3-{3-[{[(7S)-3,4-dimethoxybicyclo[4.2.0]octa-1,3,5-trien-7-yl]methyl}-(methyl)amino]propyl}-7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one Based on EP 0 534 859 A solution of the (d) camphorsulphonate salt obtained in Example 5 in ethyl acetate is brought to basic pH using sodium hydroxide and then the organic phase is separated off, washed, dried over Na2SO4 and evaporated. A mixture composed of 5.6 g of potassium carbonate, 2.2 g of the above amine in 100 mL of acetone and 4 g of 3-(3-iodopropyl)-7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one is then refluxed for 18 hours. The solvent is evaporated off in vacuo, and the residue is taken up in ethyl acetate and then extracted with 3N hydrochloric acid. The aqueous phase separated off is brought to basic pH using sodium hydroxide and is then extracted with ethyl acetate. After washing until neutral and drying over MgSO4, evaporation in vacuo is carried out to obtain 4.5 g of an oil which is purified on a silica column using a mixture of dichloromethane/methanol (90/10) as eluant. Yield=64%

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one, and friends who are interested can also refer to it.

Reference:
Patent; Les Laboratoires Servier; Vaysse-Ludot, Lucile; Le Flohic, Alexandre; Vaultier, Michel; Pucheault, Mathieu; Kaminski, Thomas; US8859763; (2014); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 148870-57-9, name is 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one, A new synthetic method of this compound is introduced below., Product Details of 148870-57-9

Based on EP 0 534 859 A solution of the (d) camphorsulphonate salt obtained in Example 4 in ethyl acetate is brought to basic pH using sodium hydroxide and then the organic phase is separated off, washed, dried over Na2SO4 and evaporated. A mixture composed of 5.6 g of potassium carbonate, 2.2 g of the above amine in 100 mL of acetone and 4 g of 3-(3-iodopropyl)-7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one is then refluxed for 18 hours. The solvent is evaporated off in vacuo, and the residue is taken up in ethyl acetate and then extracted with 3N hydrochloric acid. The aqueous phase separated off is brought to basic pH using sodium hydroxide and is then extracted with ethyl acetate. After washing until neutral and drying over MgSO4, evaporation in vacuo is carried out to obtain 4.5 g of an oil which is purified on a silica column using a mixture of dichloromethane/methanol (90/10) as eluant. Yield=64%

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; LES LABORATOIRES SERVIER; CARRANZA, Maria Del Pilar; GARCIA ARANDA, Maria Isabel; GONZALEZ, Jose Lorenzo; SANCHEZ, Frederic; US2014/107334; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 148870-57-9, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 148870-57-9 name is 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Example 6 3-{3-[{[(7S)-3,4-dimethoxybicyclo[4.2.0]octa-1,3,5-trien-7-yl]methyl}-(methyl)amino]propyl}-7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one Based on EP 0 534 859 A solution of the (d) camphorsulphonate salt obtained in Example 5 in ethyl acetate is brought to basic pH using sodium hydroxide and then the organic phase is separated off, washed, dried over Na2SO4 and evaporated. A mixture composed of 5.6 g of potassium carbonate, 2.2 g of the above amine in 100 mL of acetone and 4 g of 3-(3-iodopropyl)-7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one is then refluxed for 18 hours. The solvent is evaporated off in vacuo, and the residue is taken up in ethyl acetate and then extracted with 3N hydrochloric acid. The aqueous phase separated off is brought to basic pH using sodium hydroxide and is then extracted with ethyl acetate. After washing until neutral and drying over MgSO4, evaporation in vacuo is carried out to obtain 4.5 g of an oil which is purified on a silica column using a mixture of dichloromethane/methanol (90/10) as eluant. Yield=64%

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one, and friends who are interested can also refer to it.

Reference:
Patent; Les Laboratoires Servier; Vaysse-Ludot, Lucile; Le Flohic, Alexandre; Vaultier, Michel; Pucheault, Mathieu; Kaminski, Thomas; US8859763; (2014); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 148870-57-9, name is 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 148870-57-9, Application In Synthesis of 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one

To a mixture of (S)-N-[(4,5-dimethoxybenzocyclobut-l-yl)-methyl]-N-(methyl)amine (42g) and N,N-dimethylformamide (220ml) was charged 7,8-dimethoxy-3-[3-iodopropyl]-l,3-dihydro-2H- 3-benzazepin-2-one (75g) and potassium carbonate (42g) at room temperature. The reaction mixture was heated and stirred the reaction mass at 50-55 C for 2 hours and the completion of reaction was monitored by HPLC/TLC. After completion of reaction, reaction mass was cooled to 25-30 C and diluted with dimineralized water (1000ml). The reaction mixture was extracted with methylene dichloride (400ml x 200ml) and the layers were separated. Methylene chloride was distilled off completely. To the residue, dimineralized water (200ml) and hydrochloric acid (50ml) were added and the aqueous solution is washed with ethyl acetate (200ml x 3). The layers were separated and to the aqueous layer 50 % (w/v) sodium hydroxide solution (120ml) was added at 25-30 C. The aqueous layer was extracted with ethyl acetate (400ml + 200 ml) and the combined ethyl acetate layer was washed with 5 %( w/v) sodium hydroxide solution (300ml). Ethyl acetate layer was dried over anhydrous sodium sulfate and then ethyl acetate was distilled out completely under vacuum to get the title compound.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; IND-SWIFT LABORATORIES LIMITED; WO2008/146308; (2008); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 148870-57-9, name is 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C15H18INO3

Example 11Charge 21.0 g of [N-[[(7S)-3,4-dimethoxybicyclo[4.2.0]octa-l,3,5-trien-7-yl]methyl]-N- methylamine (V), 43.15 g of 3-(3-iodopropyl)-7,8-dimethoxy-l,3-dihydro-2H-3- benzazepine-2-one (XII), 60.0 g of K2CO3 and 315 ml of DMF in a RB flask equipped with mechanical stirrer and thermometer pocket at 25C. Heat the reaction mixture to 40-450C and maintain at the same temperature for 12 hours. Monitor the reaction by HPLC. (if starting material i.e. compound (V) remains, add compound (XII) and continue heating with stirring till compound (V) comes to less than 1.0%). If HPLC complies, cool the reaction mixture to 25C. Charge 1500 ml of IN HCl (pH should be acidic), 1500 ml of ethyl acetate (3 x 500 ml) and stir for 10 minutes and separate the layers. Charge 10% NaOH solution to aqueous layer till pH of the solution becomes basic (pH ~ 7.0 – 8.0). Charge ethyacetate (2 x 500.0 ml), stir for 10 minutes and separate the layers. Wash the ethyl acetate layer with 500 ml of water. Dry ethyl acetate layer over anhydrous Na2SO4 and evaporate ethyl acetate under vacuum at below 50C to result a brown colored residue (XIII). Weight: 43.0 gYield: 91.0 %HPLC purity (Reverse phase): >98.5%

According to the analysis of related databases, 148870-57-9, the application of this compound in the production field has become more and more popular.

148870-57-9, name is 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. category: iodides-buliding-blocks

A mixture of (8)-N- [(4,5-dimethoxybenzocyclobut- 1 -yl)methyl] -N-(methyl)amine hydrochloride (50.36g) and dimethyl formamide (200mL) ws stirred for about 5mm andpotassium carbonate (178.46g) was added to it. The reaction mixture was stirred for about lh at about room temperature. The reaction mixture was cooled to about 5C to about 10C. 7,8-dimethoxy-3 -[3-iodopropyl]- 1,3 -dihydro-2H-3 -benzazepin-2-one (I 00g) prepared as in Example 8, was added to the stirred reaction mixture. The reaction mixture was stirred for about 6h at about 20C to about 25C. The reaction mixture was quenchedinto chilled demineralized water at about 5C to about 10C. The reaction mixture was acidified to pH of about I to about 2 using concentrated hydrochloric acid and ethyl acetate was added to it. The reaction mixture was stirred and the two layers were separated. The aqueous layer was basified to pH of about 8 to about 9.5 using 20-25% aqueous ammonia solution and ethyl acetate was added to it. The reaction mixture wasstirred and the two layers were separated. The organic layer was treated with activated charcoal, stirred at about room temperature for about 30mm, filtered over hyflo bed and washed with ethyl acetate.To the above ethyl acetate layer, was added 10% palladium charcoal (15g) and the reaction mixture was hydrogenated in an autoclave under hydrogen pressure of about8kg/cm3 to about IOkg/cm?at about 65C to about 70C for about 6h. After completion of reaction, the reaction mixture is cooled to about 20C to about 25Cand filtered overhyflo bed. The hyflo bed was washed with ethyl acetate. The reaction mixture was concentrated at about below 50C under reduced pressure and acetonitrile (400mL) and isopropyl alcohol hydrogen chloride (IPA-HCI) (3OmL) was added to it at about 5C toabout 10C. The reaction mixture was stirred at about 10C to about 15C for about 3h. The reaction mixture was concentrated at about below 50C under reduced pressure and acetonitrile (400mL) was added to it. The reaction mixture was heated to about 80C to about 85C and stirred at about the same temperature for about lh. The reaction mixture was cooled and the solid obtained was filtered, washed with acetonitrile and dried at about 50C to about 55C.Yield: 85%; 1-IPLC purity: > 98%

The synthetic route of 148870-57-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLENMARK PHARMACEUTICALS LIMITED; GLENMARK GENERICS LIMITED; BHIRUD, Shekhar Bhaskar; BHUSHAN, Kumar Hari; ZOPE, Sunil Sudhakar; PATIL, Dipak Vinayak; DHEBADE, Pramod Amrutrao; CHAND, Prem; WO2014/102827; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 148870-57-9 as follows. Formula: C15H18INO3

EXAMPLE 7 3-{3-[{[(7S)-3,4-dimethoxybicyclo[4.2.0]octa-1,3,5-trien-7-yl]methyl}-(methyl)amino]propyl}-7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one Based on EP 0 534 859 A solution of the (d) camphorsulphonate salt obtained in Example 6 in ethyl acetate is brought to basic pH using sodium hydroxide and then the organic phase is separated off, washed, dried over Na2SO4 and evaporated. A mixture composed of 5.6 g of potassium carbonate, 2.2 g of the above amine in 100 mL of acetone and 4 g of 3-(3-iodopropyl)-7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one is then refluxed for 18 hours. The solvent is evaporated off in vacuo, and the residue is taken up in ethyl acetate and then extracted with 3N hydrochloric acid. The aqueous phase separated off is brought to basic pH using sodium hydroxide and is then extracted with ethyl acetate. After washing until neutral and drying over MgSO4, evaporation in vacuo is carried out to obtain 4.5 g of an oil which is purified on a silica column using a mixture of dichloromethane/methanol (90/10) as eluant. Yield=64%

According to the analysis of related databases, 148870-57-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; LES LABORATOIRES SERVIER; CARRANZA, Maria Del Pilar; GARCIA ARANDA, Maria Isabel; GONZALEZ, Jose Lorenzo; SANCHEZ, Frederic; US2014/128598; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

148870-57-9, name is 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Recommanded Product: 148870-57-9

Based on EP 0 534 859 [0053] A solution of the (d) camphorsulphonate salt obtained in Example 4 in ethyl acetate is brought to basic pH using sodium hydroxide and then the organic phase is separated off, washed, dried over Na2SO4 and evaporated. [0054] A mixture composed of 5.6 g of potassium carbonate, 2.2 g of the above amine in 100 mL of acetone and 4 g of 3-(3-iodopropyl)-7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one is then refluxed for 18 hours. [0055] The solvent is evaporated off in vacuo, and the residue is taken up in ethyl acetate and then extracted with 3N hydrochloric acid. [0056] The aqueous phase separated off is brought to basic pH using sodium hydroxide and is then extracted with ethyl acetate. After washing until neutral and drying over MgSO4, evaporation in vacuo is carried out to obtain 4.5 g of an oil which is purified on a silica column using a mixture of dichloromethane/methanol (90/10) as eluant. [0057] Yield=64%

The synthetic route of 148870-57-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; LES LABORATOIRES SERVIER; CARRANZA, Maria Del Pilar; GARCIA ARANDA, Maria Isabel; GONZALEZ, Jose Lorenzo; SANCHEZ, Frederic; US2014/163220; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com