Author: Jessica.F

Synthetic Route of 112-26-5, 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. 112-26-5, name is 1,2-Bis(2-chloroethoxy)ethane belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: In a 50 mL round bottom flask imidazole (32 mmol, 2.176 g) and potassium hydroxide (32 mmol, 1.792 g) were dissolved in DMSO (25 mL). The mixture was stirred at 70 for 1 h. After this time, 1,1?-oxybis(2-chloro-ethan (16 mmol, 1.88 ml) was added into the solution and stirred for 24 h under nitrogen atomosphere to complete the reaction which was monitored by TLC. The resulting mixture was poured into 100 mL of water and extracted with methylene chloride (5×20 mL). The combined organic layer was washed with water (3×20mL), dried over Na2SO4 and concentrated to give the crude product, which was further purified by column chromatography over silica gel using CH2Cl2 as eluent to give 1a as a pale yellow viscous oil (2.04 g, Yield = 62% ).

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, 1,2-Bis(2-chloroethoxy)ethane, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Zhou, Ji; Yuan, Yao-Feng; Zhuo, Ji-Bin; Lin, Cai-Xia; Tetrahedron Letters; vol. 59; 11; (2018); p. 1059 – 1064;,
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. 26487-67-2, name is 1-(2-Chloroethyl)azepane hydrochloride, A new synthetic method of this compound is introduced below., Formula: C8H17Cl2N

To a solution of 1,1-bis(4-hydroxyphenyl)cyclohexane (50.0 mg, 0.186 mmol) in DMF (1.86 mL) at 0 °C was added 60percent sodium hydride (dispersion in paraffin liquid, 44.7 mg, 1.12 mmol). The reaction mixture was stirred for 15 min at 50 °C and then N-(2-chloroethyl)hexahydro-1H-azepine hydrochloride (122 mg, 0.616 mmol) was added in portions at room temperature. After the reaction mixture had been stirred for 23 h at 50 °C, saturated aqueous ammonium chloride was added at 0 °C. The mixture was extracted with dichloromethane and the organic layer was dried over sodium sulfate. After filtration of the mixture and evaporation of the solvent, the crude product was purified by thin layer chromatography on silica (eluant; ammoniacal chloroform/methanol = 9/1) to afford RID-F-S*103 (compound 29) (62.7 mg, 65percent) as an orange oil

The synthetic route of 26487-67-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Hasegawa, Makoto; Yasuda, Yukari; Tanaka, Makoto; Nakata, Kenya; Umeda, Eri; Wang, Yanwen; Watanabe, Chihiro; Uetake, Shoko; Kunoh, Tatsuki; Shionyu, Masafumi; Sasaki, Ryuzo; Shiina, Isamu; Mizukami, Tamio; European Journal of Medicinal Chemistry; vol. 71; (2014); p. 290 – 305;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 6775-78-6, These common heterocyclic compound, 6775-78-6, name is 6-Chloroimidazo[1,2-b]pyridazine, 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.

478 mg (3.11 mmol) of 6-chloroimidazo[1 ,2-b]pyridazine were introduced into 10 mL of chloroform under argon and, while cooling in ice, 664 mg (3.73 mmol) of N-bromosuccuinimide were added. After the addition was complete, the reaction mixture was stirred at room temperature overnight. The reaction mixture was then mixed with water and ethyl acetate and, after addition of saturated sodium bicarbonate solution, the phases were separated. The aqueous phase was extracted three more times with ethyl acetate. The combined organic phases were then washed with sat. sodium chloride solution and dried over sodium sulfate. In the final removal of the solvent in vacuo, the desired product was isolated in quantitative yield in the form of an amorphous white solid which was employed without further chromatographic purification in subsequent reactions. 1H-NMR (CHLOROFORM-d): delta [ppm] = 7.12 (1 H); 7.79 (1 H); 7.90 (1 H).

Statistics shows that 6-Chloroimidazo[1,2-b]pyridazine is playing an increasingly important role. we look forward to future research findings about 6775-78-6.

Reference:
Patent; BAYER INTELLECTUAL PROPERTY GMBH; EIS, Knut; PUeHLER, Florian; ZORN, Ludwig; SCHULZE, Volker; SUeLZLE, Detlev; LIENAU, Philip; HAeGEBARTH, Andrea; PETERSEN, Kirstin; BOeMER, Ulf; WO2013/144189; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 15205-11-5, name is 2-Chloro-4-fluorobenzylamine, molecular formula is C7H7ClFN, 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. HPLC of Formula: C7H7ClFN

To a solution of 3,4-diflorobenzoyl chloride (45 mL, 358 mmol) in acetonitrile (1.43 L) was added solid potassium thiocyanate (KNCS) (38.2 g, 393 mmol). The suspension was stirred to 0 C for 10 min and then the cooling bath was removed. The suspension was stirred at room temperature for an additional 20 min. A solution of 2-chloro-4-fluorobenzylamine (57.1 g, 358 mmol) in acetonitrile (150 mL) was added over 5 minutes. The resulting suspension was stirred at room temperature for 3 hours. The reaction mixture was diluted with water (1.4 L) and stirred for 1 hour. The suspension was filtered, rinsed with water (150 mL) and dried in vacuo at 60 C to afford N-((2-chloro-4-fluorobenzyl)carbamothioyl)-3,4- difluorobenzamide as a yellow solid (98.3 g, 77% yield). 1HNMR (400 MHz, DMSO-d6) delta 11.56 (bs, IH), 11.12 (t, IH, J=5.7Hz), 8.00 (m, IH), 7.79 (m, IH), 7.54 (m, IH), 7.44 (m, 2H), 7.19 (m, IH), 4.85 (d, 2H, J= 5.7 Hz)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 15205-11-5, its application will become more common.

Reference:
Patent; LYCERA CORPORATION; GLICK, Gary D.; HURD, Alexander R.; TAYLOR, Clarke B.; VANHUIS, Chad A.; WO2012/78874; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 2163-00-0, The chemical industry reduces the impact on the environment during synthesis 2163-00-0, name is 1,6-Dichlorohexane, I believe this compound will play a more active role in future production and life.

Example 4; A nitrogen-purged stirred 2 l four-necked flask apparatus with internal thermometer, reflux condenser with bubble counter and pH electrode was initially charged with 136.5 g (0.55 mol) of sodium thiosulphate pentahydrate and 300 g of deionized water. The stirrer was switched on. After the thiosulphate had dissolved, 38.8 g (0.25 mol) of 1,6-dichlorohexane were added. The weakly acidic mixture was adjusted to pH 7.2+/-0.1 with 2.5% sodium hydroxide solution. The reaction vessel was purged once again briefly with nitrogen and the mixture was then boiled at reflux for 9 h, and the pH of the reaction mixture was kept at 7.2+/-0.1 during this time by addition of 2.5% sodium hydroxide solution by means of a metering pump (control by means of pH electrode). After in each case 6 and 8 hours of the reaction, the bubble counter was removed briefly from the reflux condenser. In each case approx. 5 ml of demineralized water were then sprayed with a wash bottle into the reflux condenser from the top in order to flush back into the flask any 1,6-dichlorohexane which has not dripped back. After the reaction time had ended, approx. 15 ml of 2.5% sodium hydroxide solution were used for pH control. After brief cooling, a small sample was taken from the reaction mixture to determine the conversion of 1,6-dichlorohexane by gas chromatography (GC). The GC analysis with internal standard gave a residual content of 1,6-dichlorohexane <10 ppm, which corresponds to a conversion of 1,6-dichlorohexane of >99.9%. The reaction mixture cooled to room temperature was admixed with 21.0 g (0.25 mol) of aqueous formaldehyde solution (36-38%), 21.0 g (0.25 mol) of sodium hydrogencarbonate and 43.3 g of toluene (25 parts by weight based on 100 parts by weight of the theoretically expected yield of 1,6-bis(N,N-dibenzylthiocarbamoyldithio)hexane). The headspace of the reactor was purged once again briefly with nitrogen. As soon as the hydrogencarbonate had dissolved, the feed of 773.3 g (0.5 mol) of sodium dibenzyldithiocarbamate solution (NaBEC solution) (19.1%) which had a temperature of approx. 22 C. was commenced at an internal reactor temperature of approx. 23 C. During the uniform feeding of the NaBEC solution over 1 h, the internal reactor temperature was kept at approx. 23 C. On completion of feeding, the mixture was stirred at approx. 23 C. for a further 22 h. Immediately before the commencement of the NaBEC feeding, the pH was approx. 8.3. On commencement of the NaBEC feeding, the pH rose very sharply and attained a value of approx. 10.7 at the end of the NaBEC feeding. At the end of the continued stirring time, the pH was likewise approx. 10.7. It was possible to isolate the precipitated solid very readily by suction filtration. The product was washed on the suction filter with a total of 2 1 of demineralized water in portions, which proceeded very easily. The product was dried at 50 C. and approx. 150 mbar in a vacuum drying cabinet to constant weight. The yield was approx. 91% of theory based on 1,6-dichiorohexane used. The content of 1,6-bis(N,N-dibenzylthiocarbamoyldithio)hexane was determined to be approx. 96% by means of HPLC (external standard). The melting point was approx. 92 C. The ignition residue (750 C./2 h) of the product was approx. 0.2% by weight.

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, 1,6-Dichlorohexane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Buding, Hartmuth; Weidenhaupt, Hermann-Josef; Jeske, Winfried; Kleiner, Thomas; US2005/272933; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 622-86-6, name is (2-Chloroethoxy)benzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C8H9ClO

Example 1233-{[(frans-4-Methylcyclohexyl)carbonyl][2-(phenyloxy)ethyl]amino}-1-(4-pyrazolo[1,5- a]pyrimidin-2-ylphenyl)-1H-pyrazole-4-carboxylic acidTo Intermediate 119 (200 mg) was added anhydrous DMF (8 mL), and the resulting suspension was stirred at room temperature, under nitrogen for 5 minutes. Sodium hydride (60% dispersion in mineral oil) (34 mg) was then added, and the reaction mixture stirred at room temperature, under nitrogen for 25 minutes. Beta-chlorophenetole (331 mg) was added, and the reaction was stirred at 5O0C, under nitrogen for 20 h. Water (2 mL) was added to quench the reaction, and the mixture was stirred for 15 minutes before the solvent was removed by evaporation. The residue was then suspended in THF (2 mL) and ethanol (2 mL), and 2M lithium hydroxide solution (2 mL) was then added. The reaction mixture was stirred at room temperature for 24 h, and then neutralised using 2M HCI, and partitioned between water and DCM. The layers were stirred for 30 minutes, and then separated using a hydrophobic frit. The organic phase was then concentrated by evaporation, and purified using ISCO Companion C18 chromatography eluting with a gradient of acetonitrile (containing 0.05% formic acid) in water ( containing 0.1% formic acid) to give the title compound. MS calcd for (C32H32N6O4+H)+: 565 MS found (electrospray): (M+H)+= 565

The synthetic route of 622-86-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2007/39146; (2007); 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. 29671-92-9, name is Carbamimidic chloride hydrochloride, A new synthetic method of this compound is introduced below., COA of Formula: CH4Cl2N2

The mixture of compound 1 (50 g, 0.318 mol), compound 2 (54.86 g, 0.477 mol) and methylsulfonylmethane (150.6 g, 1.59 mol) was refluxed overnight, cooled and evaporated. The resulting residue was washed mixture EtOAc-iPrOH (1 : 2). The yield was 41.65 g (0.249 mol, 78%).

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; SHY THERAPEUTICS LLC; HADARI, Yaron R.; CARTA, Luca; SCHMERTZLER, Michael; WILLIAMS, Theresa M.; REYNOLDS, Charles H.; HUTCHESON, Rebecca; (1452 pag.)WO2018/237084; (2018); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 75717-77-0, name is 2,4-Dichlorophenylacetylene, 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: C8H4Cl2

Was added quinoline (65 ~ 84.5mg, 0.5 ~ 0.65mmol) in a round bottom flask, 2,3-dichlorobenzene acetylene (85mg, 0.5mmol), trifluoromethyl propiolate (114mg, 0.75mmol), cuprous iodide (9.5mg, 10% mol), dichloromethane(5mL) as a solvent, at room temperature for 24 to 30 hours; then spin dry instead of dimethyl sulfoxide as solvent, was added copper bromide (11.2mg, 10% mol), 4- dimethylaminopyridine (12.2mg, 20% mol) 100 ~ 120 after heating the reaction to 18 to 24 hours,After cooling to room temperature with saturated brine and extracted three times with ethyl acetate, the organic layers were spin-dry column chromatography to give the pure productionThereof. As a pale yellow solid. Yield 52%.

The synthetic route of 2,4-Dichlorophenylacetylene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shanghai University; Xu, Zhiliang; Chen, Jie; Han, Jing; Zhang, Hui; Cao, Weiguo; (19 pag.)CN105669667; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 1435-48-9, A common heterocyclic compound, 1435-48-9, name is 2,4-Dichloro-1-fluorobenzene, molecular formula is C6H3Cl2F, 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 2,4-Dichloro-1-fluorobenzene (8.0 g, 48.5 mmol) in THF (63 mL) n-BuLi (23.27 mL, 2.5 M, 43.6 mmol) was added dropwise at -78 C and stirred for 1.5 h. To the mixture Sulfur (3.1 g, 72.7 mmol) was added at -78 C and stirring for 2 h. To the resulting mixture 10% Hydrochloric acid (HCl) was added to adjust pH to 5-6. The resulting mixture was extracted with EtOAc (200 mL * 3), the combined organic phase was washed with brine (100 mL * 2), dried over Na2SO4. After filtered, the organic phase was concentrated to dry to give compound 31 as yellow oil (11.4 g, 99.0% yield). 1H NMR (400 MHz, CDCl3) delta 7.31-7.19 (m, 1H, Ar-H), 6.95-6.89 (t, 1H, Ar-H), 4.69 (s, 1H, SH).

The synthetic route of 1435-48-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Liu, Na; Wang, Yanfen; Huang, Gongchao; Ji, Conghui; Fan, Wei; Li, Haitao; Cheng, Ying; Tian, Hongqi; Bioorganic Chemistry; vol. 65; (2016); p. 146 – 158;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 13918-92-8, The chemical industry reduces the impact on the environment during synthesis 13918-92-8, name is 2,4-Difluorobenzene-1-sulfonyl chloride, I believe this compound will play a more active role in future production and life.

General procedure: Compound 11a (800 mg,2.0 mmol) was dissolved in 10 ml ethyl acetate and then 9 N HCl(5 ml) was added, the reaction mixture was stirred for 30 min at roomtemperature, the reaction solvent was neutralized by NaHCO3 topH=8, 50 ml ethyl acetate and 30 ml H2O was added, after stirredadequately, the organic layer was separated, and concentrated, andthen the crude product was purified by silica gel columnchromatography using a mixture solvent of dichloromethane:methanol (20:1), to give white powder (540 mg); Above whitepowder (150 mg, 0.5 mmol) was dissolved in THF (10 ml),iodomethane (107 mg, 0.75 mmol) and triethylamine (0.5 ml) wereadded in the solvent. After the reaction mixture was stirred for 1 h at room temperature, the solvent was concentrated, the residues was purified by silica gel column chromatography using a mixture solvent ofdichloromethane: methanol (40:1), to give (12aa) Yield 49%, White powder.

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, 2,4-Difluorobenzene-1-sulfonyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Zhang, Min; Jiang, Li; Tao, Jia; Pan, Zhaoping; He, Mingyao; Su, Dongyuan; He, Gu; Jiang, Qinglin; Bioorganic and Medicinal Chemistry; vol. 27; 11; (2019); p. 2268 – 2279;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics