Category: 876-53-9

Electric Literature of 876-53-9, 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 876-53-9 as follows.

EXAMPLE II Preparation of 1,3-bis(2,2-dibromoethyl)adamantane. A solution of 147 g (0.5 mol) of 1,3-dibromoadamantane and 300 ml (3 mol) of vinyl bromide in 250 ml of methylene chloride was stirred and cooled to -20 C. in an ice-methanol bath and then 25 g (0.094 mol) of aluminum bromide was added portionwise over 1 h. The mixture was stirred for 2 h. during which time the temperature was allowed to rise to ambient. The solution was washed with 100 ml of water, 250 ml of concentrated aqueous hydrochloric acid, and 100 ml of water, drived (MgSO4) and evaporated to give 292 g of an oil. This material contained 1,3-bis(2,2-dibromoethyl)-adamantane and polyvinyl bromide, and was used without further purification.

According to the analysis of related databases, 876-53-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Baum; Kurt; Archibald; Thomas G.; US4849565; (1989); A;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 876-53-9, name is 1,3-Dibromoadamantane, A new synthetic method of this compound is introduced below., Application In Synthesis of 1,3-Dibromoadamantane

A compound of 1,3-dibromo-adamantane (3 g, 10 mmol) was dissolved in 30 mL of toluene, and then 250 mg of AIBN (1.5 mmol), 7 g of tri-n-butyl tin (24 mmol), 3 g of 2-ethyl methacrylate were added in order. The reaction was refluxed at 110 C. under nitrogen for 3 hours. The reaction solution was cooled to room temperature, and was poured into 30 mL of 0.2 M aqueous ammonia. After being stirred fully, the organic layer was separated, the aqueous layer was extracted with ethyl acetate (20 mL×4). The organic layers were combined, and washed with 30 mL of water and 30 mL of saturated sodium chloride solution, dried with anhydrous sodium sulfate. The solvent was evaporated under reduced pressure to give a crude product as a colorless oil, which was separated by silica column chromatography (petroleum ether:ethyl acetate=10:1) to obtain NM-012a as a colorless oil (1.6 g, 43.1%). ESI-MS: m/z 337.4 ([M+H]+). 1H-NMR (DMSO-d6, ppm): 0.97 (s, 2H), 1.02-1.08 (m, 8H), 1.15-1.20 (m, 7H), 1.22-1.40 (m, 7H), 1.50 (s, 2H), 1.57-1.65 (m, 2H), 1.93 (s, 2H), 2.39-2.47 (m, 2H), 3.98-4.11 (m, 4H).

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; Guangzhou Magpie Pharmaceuticals Co., Ltd.; Wang, Yuqiang; Liu, Zheng; Yu, Pei; Sun, Yewei; Zhang, Zaijun; Zhang, Gaoxiao; Shan, Luchen; Yi, Peng; Larrick, James; (19 pag.)US2018/148404; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 876-53-9, name is 1,3-Dibromoadamantane, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C10H14Br2

General procedure: In a stainless-steelpressure microreactor of 17 mL capacity was charged5 wt % of catalyst FeHY (or NiHY), 100 mmol ofhaloadamantane (or halodiadamantane), and 400 mmolof dimethyl carbonate, the reactor was tightly closed,and the reaction mixture was heated for 5 h at 150.On completing the reaction, the reactor was cooled toroom temperature, opened, the reaction mixture wasfiltered through a layer of Al2O3. The unreacteddimethyl carbonate was distilled off

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 876-53-9.

Reference:
Article; Khusnutdinov; Shchadneva; Mayakova, Yu. Yu.; Russian Journal of Organic Chemistry; vol. 54; 11; (2018); p. 1728 – 1730; Zh. Org. Khim.; vol. 54; 9; (2018); p. 1710 – 1712,3;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 876-53-9,Some common heterocyclic compound, 876-53-9, name is 1,3-Dibromoadamantane, molecular formula is C10H14Br2, 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.

Compound 1,3-dibromo-adamantane (3 g, 10 mmol) was dissolved in 30 mL of toluene, and then 250 mg ofAIBN (1.5 mmol), 7 g of tri-n-butyl tin (24 mmol), 3 g of ethyl acrylate (30 mmol) were added in order. The reaction wasrefluxed with at 110 C under nitrogen for 3 hours. The reaction solution was cooled to room temperature and was pouredinto 30 mL of 0.2M aqueous ammonia. After being stirred fully, the organic layer was separated. The aqueous layerswere extracted with ethyl acetate (20 mL34). The organic layers were combined and washed with 30 mL of water and30 mL of saturated sodium chloride solution. The resulting materials were dried with anhydrous sodium sulfate, andsolvent was evaporated under the reduced pressure to give a crude product as a colorless oil, which was separated bysilica column chromatography (petroleum ether : ethyl acetate = 10:1) to give compound NM-011a as a colorless oil (2g, 46.6%). ESI-MS: mlz 337.4 ([M+H]+). 1H-NMR (DMSO-d6, ppm): 1.11 (s, 2 H), 1.15-1.19 (m, 6 H), 1.28-1.39 (m, 12H), 1.53 (s, 2 H), 1.97 (s, 2 H), 2.19-2.24 (m, 2 H), 4.03 (q, 4 H, J=7.1 Hz).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,3-Dibromoadamantane, its application will become more common.

Reference:
Patent; Guangzhou Magpie Pharmaceuticals Co., Ltd.; WANG, Yuqiang; LIU, Zheng; YU, Pei; SUN, Yewei; ZHANG, Zaijun; ZHANG, Gaoxiao; SHAN, Luchen; YI, Peng; LARRICK, James; (27 pag.)EP3150574; (2017); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 876-53-9,Some common heterocyclic compound, 876-53-9, name is 1,3-Dibromoadamantane, molecular formula is C10H14Br2, 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.

Compound 1,3-dibromo-adamantane (3 g, 10 mmol) was dissolved in 30 mL of toluene, and then 250 mg of AIBN (1.5 mmol), 7 g of tri-n-butyl tin (24 mmol), 3 g of ethyl acrylate (30 mmol) were added in order. The reaction was refluxed with at 110 C. under nitrogen for 3 hours. The reaction solution was cooled to room temperature and was poured into 30 mL of 0.2M aqueous ammonia. After being stirred fully, the organic layer was separated. The aqueous layers were extracted with ethyl acetate (20 mL×4). The organic layers were combined and washed with 30 mL of water and 30 mL of saturated sodium chloride solution. The resulting materials were dried with anhydrous sodium sulfate, and solvent was evaporated under the reduced pressure to give a crude product as a colorless oil, which was separated by silica column chromatography (petroleum ether:ethyl acetate=10:1) to give compound NM-011a as a colorless oil (2 g, 46.6%). ESI-MS: m/z 337.4 ([M+H]+). 1H-NMR (DMSO-d6, ppm): 1.11 (s, 2H), 1.15-1.19 (m, 6H), 1.28-1.39 (m, 12H), 1.53 (s, 2H), 1.97 (s, 2H), 2.19-2.24 (m, 2H), 4.03 (q, 4H, J=7.1 Hz).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,3-Dibromoadamantane, its application will become more common.

Reference:
Patent; Guangzhou Magpie Pharmaceuticals Co., Ltd.; Wang, Yuqiang; Liu, Zheng; Yu, Pei; Sun, Yewei; Zhang, Zaijun; Zhang, Gaoxiao; Shan, Luchen; Yi, Peng; Larrick, James; (19 pag.)US2018/148404; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 876-53-9, 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 876-53-9 as follows.

EXAMPLE II Preparation of 1,3-bis(2,2-dibromoethyl)adamantane. A solution of 147 g (0.5 mol) of 1,3-dibromoadamantane and 300 ml (3 mol) of vinyl bromide in 250 ml of methylene chloride was stirred and cooled to -20 C. in an ice-methanol bath and then 25 g (0.094 mol) of aluminum bromide was added portionwise over 1 h. The mixture was stirred for 2 h. during which time the temperature was allowed to rise to ambient. The solution was washed with 100 ml of water, 250 ml of concentrated aqueous hydrochloric acid, and 100 ml of water, drived (MgSO4) and evaporated to give 292 g of an oil. This material contained 1,3-bis(2,2-dibromoethyl)-adamantane and polyvinyl bromide, and was used without further purification.

According to the analysis of related databases, 876-53-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Baum; Kurt; Archibald; Thomas G.; US4849565; (1989); A;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 876-53-9, name is 1,3-Dibromoadamantane, 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. COA of Formula: C10H14Br2

A compound of 1,3-dibromo-adamantane (3 g, 10 mmol) was dissolved in 30 mL of toluene, and then 250 mgof AIBN (1.5 mmol), 7 g of tri-n-butyl tin (24 mmol), 3 g of 2-ethyl methacrylate were added in order. The reaction wasrefluxed at 110C under nitrogen for 3 hours. The reaction solution was cooled to room temperature, and was poured into 30 mL of 0.2 M aqueous ammonia. After being stirred fully, the organic layer was separated, the aqueous layer wasextracted with ethyl acetate (20 mL34). The organic layers were combined, and washed with 30 mL of water and 30mL of saturated sodium chloride solution, dried with anhydrous sodium sulfate. The solvent was evaporated underreduced pressure to give a crude product as a colorless oil, which was separated by silica column chromatography(petroleum ether : ethyl acetate = 10:1) to obtain NM-012a as a colorless oil (1.6 g, 43.1%). ESI-MS: m/z 337.4 ([M+H]+). 1H-NMR (DMSO-d6, ppm): 0.97 (s, 2 H), 1.02-1.08 (m, 8 H), 1.15-1.20 (m, 7 H), 1.22-1.40 (m, 7 H), 1.50 (s, 2 H),1.57-1.65 (m, 2 H), 1.93 (s, 2 H), 2.39-2.47 (m, 2 H), 3.98-4.11 (m, 4 H).

The synthetic route of 1,3-Dibromoadamantane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Guangzhou Magpie Pharmaceuticals Co., Ltd.; WANG, Yuqiang; LIU, Zheng; YU, Pei; SUN, Yewei; ZHANG, Zaijun; ZHANG, Gaoxiao; SHAN, Luchen; YI, Peng; LARRICK, James; (27 pag.)EP3150574; (2017); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 876-53-9,Some common heterocyclic compound, 876-53-9, name is 1,3-Dibromoadamantane, molecular formula is C10H14Br2, 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.

In a 250 ml round bottom flask, 1,3-dibromoadamantane (15 mmol), cuprous oxide (40 mmol), and DMAC (20 ml) were refluxed for 48 hours under an argon atmosphere.The obtained intermediate was cooled to room temperature, added to water, then filtered through a pad of Celite, and the filtrate was extracted with dichloromethane.The organic phase was then washed with water and the organic phase was dried over anhydrous magnesium sulfate.After filtering and evaporating the organic phase, the crude product was purified by silica gel column chromatography.The intermediate product H14-1 was obtained.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,3-Dibromoadamantane, its application will become more common.

Reference:
Patent; Shanghai Tianma Organic Shine Display Co., Ltd.; Dai Wenpeng; Gao Wei; Niu Jinghua; Zhang Lei; Lu Yan; Deng Dongyang; (40 pag.)CN110156756; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 876-53-9, 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 876-53-9 as follows.

General procedure: A solution of 43 g (0.2 mol) of 1-bromoadamantane in 260 mL of methylene chloride was cooled to -10 C, and 61.9 g (0.23 mol) of aluminum bromide was added. The mixture was stirred for 0.5 h, 44 mL (40 g, 0.42 mol) of isopropenyl acetate was added over a period of 2 h, and the mixture was stirred for 0.5 h, poured onto 200 g of ice, and made weakly alkaline reaction by adding sodium carbonate (106 g, 1 mol) and sodium metabisulfite (38 g, 0.2 mol). The organic layer was separated, and the aqueous layer was extracted with methylene chloride (3 ¡Á 50 mL). The extracts were combined with the organic phase, the solvent was distilled off, and the residue was distilled under reduced pressure. Yield 31.9 g (83%), bp 110-112 C (4 mm). 1H NMR spectrum (DMSO-d6), delta, ppm: 1.50-1.80 m (12H, CH2), 1.94 s (3H, CH), 2.10 s (3H, CH3), 2.16 s (2H, CH2CO).

According to the analysis of related databases, 876-53-9, the application of this compound in the production field has become more and more popular.

Reference:
Article; Novakov; Orlinson; Savel?ev; Potaenkova; Vostrikova; Tarakanov; Nakhod; Russian Journal of General Chemistry; vol. 87; 12; (2017); p. 2762 – 2765; Zh. Obshch. Khim.; vol. 87; 12; (2017); p. 1942 – 1946,5;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 876-53-9, name is 1,3-Dibromoadamantane, belongs to bromides-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 876-53-9, 876-53-9

1. Under nitrogen protection, 440 g of 1,3-dibromoadamantane was added to a 10 L four-necked flask. Then 2.0 L of dichloroethane was added and stirred well, 500 g of acetanilide was added and stirred well. Add zinc dichloride slowly and stir it well, then heat up to reflux (internal temperature 80-85C). Partially separate the water with a water separator and then use a reflux device. After refluxing at this temperature for 24 hours, the lower layer was a viscous solid and the upper layer was a dichloroethane solvent. Cool to room temperature, pour off the upper layer of solvent, add 1.0L DMF (N,N-dimethylformamide) to raise the temperature to a solid slurry, and slowly pour the slurry into 4.0L of stirring water. Stir 30%. Filter after minutes The solid crude product was obtained in a wet weight of 1219 g. The solid was added to 6 L of water for beating for 3.5 hours, filtered and pumped until no liquid was dripped, and then washed with water (2¡Á2 L). 1332 g of crude wet weight was obtained, refluxed with two-fold volume of ethanol (3 L) for 1 hour, cooled to room temperature and stirred at room temperature for 1 hour, filtered to dry wet weight 522 g and used directly for the second reaction.

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, 1,3-Dibromoadamantane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Shanghai Bodong Chemical Technology Co., Ltd.; Fu Zhiwei; He Baoyuan; Pan Xingang; Yu Wenqing; Li Yongli; Lu Wei; (7 pag.)CN107673977; (2018); A;,
Bromide – Wikipedia,
bromide – Wiktionary