Category: 148870-57-9

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: 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one

A mixture of the iodo-compound of formula (III) (50.00 g; 129 mmol), amine hydrochloride of formula (IV) (31.50 g; 129 mmol), potassium carbonate (37.70 g; 273 mmol), toluene (80 ml) and water (40 ml) was heated to 70C with stirring under an argon atmosphere. Reaction progress was monitored by HPLC. Upon completion, the reaction mixture was cooled to 23 C, diluted with toluene (105 ml), and filtered through a pad of celite. The filter cake was washed with additional toluene (60 ml). To the filtrate, water (50 ml) was added, and the mixture was shaken. The organic layer was separated and washed with additional water (80 ml). The separated organic layer was then extracted with 9% aqueous hydrochloric acid (507 g) in three portions. Yield of dehydroivabradine hydrochloride in combined acidic extracts was calculated based on HPLC assay using an external standard. The product was obtained in 80% yield as an aqueous solution which was used directly in the next step.

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

Reference:
Patent; SYNTHON BV; MEL?A, Petr; ZABADAL, Miroslav; WO2014/114341; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 148870-57-9, The chemical industry reduces the impact on the environment during synthesis 148870-57-9, name is 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one, I believe this compound will play a more active role in future production and life.

From 11 g of that product, 3.3 g of LiAlH4 and 160 ml of tetrahydrofuran heated at reflux for 6 hours, 7 g of N-[(4-methoxybenzocyclobut-1-yl)methyl)-N-(methyl)amine (yield 90%) are obtained. From 15 g of 7,8-dimethoxy-3-[3-iodopropyl]-1,3-dihydro-2H-3-benzazepin-2-one, 7 g of N-[(4-methoxybenzocyclobut-1-yl)methyl]-N-(methyl)amine, 22 g of K2 CO3 and 300 ml of acetone, there are obtained 17.5 g (theoretical yield) of 7,8-dimethoxy-3-{3-{N-[(4-methoxybenzocyclobut-1-yl)-methyl)-N-(methyl)amino}propyl}-1,3-dihydro-2H-3-benzazepin-2-one. From 5 g of that product, 60 ml of ethanol, 1 ml of acetic acid and 3 g of palladium hydroxide, there are obtained 1.9 g of 7,8-dimethoxy-3-{3-{N-[(4-methoxybenzocyclobut-1-yl)methyl]-N-(methyl)amino}propyl}-1,3,4,5-tetrahydro-2H-3-benzazepin.-2-one (yield: 65%), which is converted into the corresponding dihydrochloride which, recrystallized from acetonitrile, melts at 160-164 C.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Adir et Compagnie; US5296482; (1994); A;,
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, 148870-57-9

7,8-Dimethoxy-3-[3-iodopropyl]-l,3-dihydro-2H-3-benzazepin-2-one (38g) and potassium carbonate (6Og) were added to a mixture of (S)-N-[(4,5-dimethoxybenzocyclobut-l-yl)-methyl]- 7V-(methyl)amine (2Og) and demineralized water (100ml) at room temperature. The reaction mixture was heated and stirred at 50-55 C for 12-16 hours. After completion of reaction, reaction mass was cooled to 25-30 0C and the product is extracted in ethyl acetate (100ml). The aqueous layer was further extracted with ethyl acetate (60ml). Combined ethyl acetate layers was acidified with aqueous hydrochloric acid and stirred. The layers were separated and pH of the aqueous layer was adjusted to 10.5-12.5 with aqueous sodium hydroxide solution. The aqueous layer is extracted with ethyl acetate (140ml + 60ml). Ethyl acetate was distilled out completely under vacuum to get the title compound.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; IND-SWIFT LABORATORIES LIMITED; WO2008/146308; (2008); A2;,
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. 148870-57-9

Example 1:Preparation of 7,8-dimethoxy-3- [3- [[(1 S)-(4,5-dimethoxybenzocyclobutan-1- yl)methyl] methylamino] propyll-1 ,3-de-hydro-7,8-dimethoxy-2H-3-benzazepin-2-one oxalate (De-hydro ivabradine oxalate salt) 3-[3-lodopropylj-7,8-dimethoxy- I H-3-benzazepin-2(3H)-one (100 gm),dimethylformamide (800 ml), potassium carbonate (140 gm) and (S)-N-[(4,5-dimethoxybenzocyclobut- 1 -yl)-methyl]-N-(methyl)amine hydrochloride (40 gm) were added and then heated to 40 to 45C. The reaction mass was maintained for 17 hours at 40 to 45C and then cooled to room temperature. To the reaction mass were added hydrochloric acid (iN, 3000 ml) and ethyl acetate (2000 ml). The layers were separatedand the aqueous layer was extracted with ethyl acetate. Combined organic layers were dried with sodium sulfate and then concentrated to obtain a residual solid. To the residual solid was added ethyl acetate (750 ml) and then added a solution of oxalic acid (27 gm) in acetone (100 ml). The reaction mass was stirred for 2 hours at room temperature and filtered. The solid obtained was dried to obtain 90 gm of de-hydro ivabradine oxalate salt.Chromatographic purity of de-hydro ivabradine oxalate salt: 96.5%.

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.

Reference:
Patent; HETERO RESEARCH FOUNDATION; PARTHASARADHI REDDY, Bandi; RATHNAKAR REDDY, Kura; MURALIDHARA REDDY, Dasari; SRINIVASA RAO, Thungathurthy; VAMSI KRISHNA, Bandi; WO2013/150544; (2013); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com