Month: September 2021

Adding a certain compound to certain chemical reactions, such as: 6306-61-2, name is N-(2-Chloroethyl)propan-2-amine hydrochloride, belongs to chlorides-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 6306-61-2, Application In Synthesis of N-(2-Chloroethyl)propan-2-amine hydrochloride

To a stirred mixture of 2-methyltetrahydrofuran (1.5L) and KOH (140g, 250mmol) was added water (30ml_). Then intermediate 3 (60g, 166mmol)) andtetrabutylammoniumbromide (13.4g, 41 mmol) were added and the mixture was heated at 50C for 1 hour while stirring. Then N-(2-chloroethyl)-2-propanamine HCI (CAS[6306- 61 -2]) (48g, 299mmol) was added in 1 portion. The mixture was stirred for 18 hours at 50C. When the conversion was complete, water (600ml_) was added to the reaction mixture. The layers were separated and the organic layer was concentrated. The residue was dissolved in 2-propanol (120ml_) and HCI in 2-propanol was added at 60C. After cooling, the HCI-salt was isolated via filtration. After drying at 50C in a vacuum drying oven the HCI-salt was obtained in 83% yield (compound 4a).

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, N-(2-Chloroethyl)propan-2-amine hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASTEX THERAPEUTICS LIMITED; SAXTY, Gordon; MURRAY, Christopher William; BERDINI, Valerio; BESONG, Gilbert Ebai; HAMLETT, Christopher Charles Frederick; JOHNSON, Christopher Norbert; WOODHEAD, Steven John; READER, Michael; REES, David Charles; MEVELLEC, Laurence Anne; ANGIBAUD, Patrick Rene; FREYNE, Eddy Jean Edgard; GOVAERTS, Tom Cornelis Hortense; WEERTS, Johan Erwin Edmond; PERERA, Timothy Pietro Suren; GILISSEN, Ronaldus Arnodus Hendrika Joseph; WROBLOWSKI, Berthold; LACRAMPE, Jean Fernand Armand; PAPANIKOS, Alexandra; QUEROLLE, Oliver Alexis Georges; PASQUIER, Elisabeth Therese Jeanne; PILATTE, Isabelle Noelle Constance; BONNET, Pascal Ghislain Andre; EMBRECHTS, Werner Constant Johan; AKKARI, Rhalid; MEERPOEL, Lieven; WO2011/135376; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 61881-19-4, name is 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 61881-19-4

Compound 4 (0.91 g, 4.09 mmol) was dissolved in 5ml acetone, and then2,2,2-trifluoro-N-phenylethanimidoyl chloride (0.87 g, 4.19 mmol) and potassiumcarbonate (0.58 g, 4.19 mmol) were successively added. After stirring at roomtemperature for about 18 h, the mixture was evaporated under reduced pressure.The residue was purified by column chromatography on silica gel (200-300 mesh) toafford pure 8, yield 87%. TLC (ethyl acetate/petroleum ether 4:1, V:V); 1H NMR (400MHz, CDCl3) delta: 1.31 (m, 3H, CH3), 1.35 (m, 3H, CH3), 3.15 (m, 1H, CH), 3.22 (m, 1H,CH), 3.50 (s, 3H, CH3), 3.59 (s, 3H, CH3), 3.61 (m, 2H, CH2), 3.69 (m, 1H, CH), 3.75(m, 1H, CH), 5.25 (s, 1H, CH); 6.88(m, 1H, CH), 7.14 (s, 1H, CH), 7.33 (m, 1H, CH),7.44 (s, 1H, CH); 7.59 (s, 1H, CH) ; 13C NMR (100 MHz, CDCl3) delta: 15.6, 17.8, 59.2,61.1, 67.8, 70.7, 79.7, 82.0, 96.2, 117.3, 119.5, 120.4, 125.4, 129.2, 129.4,133.9, 143.6; MS (ESI) cal for C18H24F3NO5 [M+Na]+ 414.14988, found [M+Na]+414.15034.

According to the analysis of related databases, 61881-19-4, the application of this compound in the production field has become more and more popular.

Reference:
Article; Zhang, Kai; Liu, Shenglan; Liu, Anjun; Chai, Hongxin; Li, Jiarong; Lamusi; Beilstein Journal of Organic Chemistry; vol. 13; (2017); p. 2603 – 2609;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 10061-02-6, A common heterocyclic compound, 10061-02-6, name is trans-1,3-Dichloropropene, molecular formula is C3H4Cl2, 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.

Eine geruehrte Loesung von 77,7 ml Diisopropylamin und 200 ml Tetrahydrofuran wird auf -20 C gekuehlt und waehrend 15 Minuten mit 200 ml 2,5 M n-Hexyllithiumloesung (in Hexan) versetzt. Die Loesung wird 15 Minuten bei -20 C nachgeruehrt und anschliessend wird waehrend 30 Minuten eine Loesung von 75,3 ml Isovaleriansaeureethylester in 80 ml Tetrahydrofuran zugetropft. Die Loesung wird 10 Minuten nachgeruehrt und dann waehrend 10 Minuten bei -20 C mit 80 ml DMPU versetzt. Zugabe von 8,2 g Natriumiodid und 19,5 g trans-1,3-Dichlorpropen. Das Reaktionsgemisch wird noch 23 Stunden bei – 20 C nachgeruehrt und anschliessend mit 500 ml 20%-iger waessriger Ammoniumchloridloesung versetzt. Die Mischung wird mit tert.-Butylmethylether (2x 400 ml) extrahiert und die organischen Phasen nacheinander mit 0,1 M Natriumthiosulfatloesung (1x 500 ml), Wasser (1x 500 ml) und Sole (1x 500 ml) gewaschen. Die vereinigten organischen Phasen werden mit 150 g Natriumsulfat getrocknet und eingedampft. Aus dem Rueckstand wird mittels Destillation die Titelverbindung A1 als farbloses Oel erhalten (86,1 g, 84 %). 1H-NMR (400 MHz, CDCl3, delta) : 0,95 (m, 6H), 1,30 (t, 3H), 1,92 (m, 1H), 2,20 – 2,40 (m, 3H), 4,20 (m, 2H), 5, 80 – 6,10 (m, 2H) ppm.

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; Speedel Pharma AG; EP1200384; (2004); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 7149-75-9, name is 4-Chloro-3-methylaniline, A new synthetic method of this compound is introduced below., Recommanded Product: 7149-75-9

General procedure: To a solution of ethyl acetoacetate (10 mmol) in 40 mL of toluene was added appropriate amine(10 mmol) and a catalytic amount of potassium tert-butoxide. The resulting mixture was heated torefluxing for 6 hours. After the reaction mixture was cooled to room temperature, the solvent wasremoved under rotovap and the crude product was purified by flash chromatography on silica gelusing hexane:EtOAc (1:1) to afford desired products as colorless crystalline solid (40%-63%).

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:
Article; Tang, Jing; Huber, Andrew D.; Pineda, Dallas L.; Boschert, Kelsey N.; Wolf, Jennifer J.; Kankanala, Jayakanth; Xie, Jiashu; Sarafianos, Stefan G.; Wang, Zhengqiang; European Journal of Medicinal Chemistry; vol. 164; (2019); p. 179 – 192;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 15205-11-5, name is 2-Chloro-4-fluorobenzylamine, belongs to chlorides-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 15205-11-5, Safety of 2-Chloro-4-fluorobenzylamine

Example 1; lambda/-[(2-chloro-4-fluorophenyl)methyl]-2-(1 ,4-dimethyl-1 H-pyrazol-5- yl)acetamide (E1); A mixture of (1 ,4-dimethyl-1 H-pyrazol-5-yl)acetic acid and (1 ,4-dimethyl-1H-pyrazol- 3-yl)acetic acid (1.2 g, 2.mmol, prepared as described below), 1- hydroxybenzotriazole hydrate (324 mg, 2.4 mmol), 1-ethyl-3-(3- dimethylaminopropyl)carbodiimide hydrochloride (460 mg, 2.4 mmol) and lambda/-ethyl morpholine (690 mg, 0.76 ml, 6 mmol) in dichloromethane (10 ml) was stirred at room temperature for 10 minutes. A solution of [(2-chloro-4- difluorophenyl)methyl]amine (319 mg, 2 mmol) in dichloromethane (1 ml) was added and the reaction stirred at room temperature for 4 hours. The reaction mixture was diluted with saturated sodium bicarbonate solution and dichloromethane. The organic layer was separated washed with water and brine, dried and evaporated. The residue was purified by column chromatography on silica gel eluting with ethyl acetate/hexane mixtures (1 :1 to neat ethyl acetate), followed by silica gel chromatography eluting with dichloromethane/methanol (40:1 ) to give lambda/-[(2-chloro-4- fluorophenyl)methyl]-2-(1 ,4-dimethyl-1 H-pyrazol-5-yl)acetamide.LC/MS [M+H]+ = 329, retention time = 2.35 minutes.

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, 2-Chloro-4-fluorobenzylamine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GLAXO GROUP LIMITED; WO2008/125600; (2008); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 94-97-3, 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. 94-97-3 name is 5-Chloro-1H-benzo[d][1,2,3]triazole, 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.

A solution of 5-chloro-1/-/-benzotriazole (1 53 g) in THF was added at 0C to a mixture of diisopropylic azodicarboxylate (2 ml_), triphenyl phosphine (2.9 g) and allyl alcohol (1.4 mL) in THF. After stirring one hour at 00C, the mixture was concentrated under reduced pressure to give a residue that was purified by chromatography (SiO2, heptane/EA) to afford 2-allyl-5-chloro-2/-/-benzotriazole (1.02 g, 53%). A mixture of 1- allyl-5-chloro-1/-/-benzotriazole and 1-allyl-6-chloro-1/-/-benzotriazole was also recovered (0.9 g, 47%). Alternatively, 2-allyl-5-chloro-2H-benzotriazole [4.87 g, 25%,Rf =0.4 (1 :3 EA/heptane)] was obtained using a procedure similar to that described in Example 1 , part a, except using 3-bromopropene. Similarly, a mixture of 1-allyl-5- chloro-1 H-benzotriazole and 1-allyl-6-chloro-1/-/-benzotriazole was also recovered [10.81 g, 56%, Rf =0.2 (1 :3 EA/heptane)]

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-Chloro-1H-benzo[d][1,2,3]triazole, and friends who are interested can also refer to it.

Reference:
Patent; MERIAL LIMITED; AVENTIS AGRICULTURE; WO2008/144275; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 121-27-7, name is 5-Chloro-2-(4-chlorophenoxy)aniline, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C12H9Cl2NO

In the reactor was added 800kg 44.45% nitrosyl sulfuric acid solution,Warmed to 25 C,The melted 700kg amino material slowly added to the reactor,The reaction was incubated at 30 ~ 35 2 hours to complete the reaction of the amino compound,

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 121-27-7.

Reference:
Patent; Jiangsu Yi Ke Chemical Co., Ltd.; Yi Jianghua; Xie Shoulei; Yu Qianli; (6 pag.)CN107353185; (2017); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 1005-56-7, name is O-Phenyl carbonochloridothioate, belongs to chlorides-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 1005-56-7, Quality Control of O-Phenyl carbonochloridothioate

General procedure: 1a (0.996g, 1.5mmol) / 1b (0.204g, 0.30mmol), NaOH (0.18g, 4.5mmol / 0.072g, 1.8mmol) in 20mL Stir in CH2Cl2 for 15 minutes. Join slowly in 5 minutesPhenyl thiochloroformate(0.258 g, 1.5 mmol / 0.103 g, 0.6 mmol).The TLC dot plate tracks the progress of the reaction and stops the reaction after the disappearance of the raw materials.10% HCl was added to the reaction solution to neutralize excess NaOH.After oscillating, the organic phase was separated and the aqueous phase was extracted with CH2Cl2.The organic phase was combined, washed with brine and dried over anhydrous sodium sulfate.After concentrating by evaporation, the crude product was purified and purified by ethylamine (ethyl acetate: petroleum ether = 1:100) to give white solid 2a (0.75 g, yield 71%) and 2b (0.171 g,Yield 75%).

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; Changzhou University; Li Zhengyi; Tong Hongxiao; Chen Yuan; Yin Le; Xiao Tangxin; Sun Xiaoqiang; (9 pag.)CN108727241; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 108649-59-8, 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. 108649-59-8 name is 1-(2-Bromoethyl)-2,4-dichlorobenzene, 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.

1- (2-BROMOETHYL)-2, 4-CHLOROBENZENE * (6.8g) was mixed with sodium sulphite (3.36g) in a 4: 1 mixture of water : dioxan (50MI) and heated to 140C overnight. A further 25ML of dioxan was added and reflux continued for a further 24 hours.. The mixture was then cooled to room temperature and concentrated in vacuo. The residue was triturated with diethyl ether and dried to give the title compound. RT 3.68min [M-Na] + 253. * Sharafian et AL., J. Het. Chem. 1994,31, 6,1421

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-(2-Bromoethyl)-2,4-dichlorobenzene, and friends who are interested can also refer to it.

Reference:
Patent; GLAXO GROUP LIMITED; WO2004/52851; (2004); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 1996-29-8, name is 1-Bromo-4-chloro-2-fluorobenzene, A new synthetic method of this compound is introduced below., Application In Synthesis of 1-Bromo-4-chloro-2-fluorobenzene

General procedure: In a 15 mL sealed tube equipped with a magnetic stirring bar were added 1 (1 mmol),2 (0.8 mmol), tert-butyl isocyanide (1.2 mmol, 136 muL), Pd(OAc)2 (0.03 mmol, 7 mg),DPEPhos (0.06 mmol, 32 mg), Cs2CO3 (0.8 mmol, 261 mg), and anhydrous DMF (2.0mL). The tube was purged with argon, and the contents were stirred at 100 C for 2 h.Then Na2S*9H2O (1.2 mmol, 240 mg) was added for 2 h. After reaction completion,the mixture was filtered through a pad of Celite, and DMF was removed by a vacuum.The combined filtrates were refluxed in THF (15 mL) and oxalic acid (1 M, 3 mL) for 8h. The solvents were removed under reduced pressure, then poured into brine (20mL) and extracted by ethyl acetate (3 × 30 mL). The combined organic layers weredried (Na2SO4) and evaporated. The residue was purified on a silica gel column usingpetroleum ether/ethyl acetate as the eluent to give the pure target product.

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:
Article; Zhang, Fang-Ling; Chen, Zhen-Bang; Liu, Kui; Yuan, Qing; Jiang, Qing; Zhu, Yong-Ming; Synlett; vol. 29; 5; (2018); p. 621 – 626;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics