Author: Jessica.F

Synthetic Route of 2268-05-5, The chemical industry reduces the impact on the environment during synthesis 2268-05-5, name is 2,6-Dichlorofluorobenzene, I believe this compound will play a more active role in future production and life.

4,4,4>,4>,5,5,5′,5′-Octamethyl[2,2′-bi-1,3,2-dioxaborolane] (10.0 g, 39.4 mmol), 2,6- bis(l-methylethyl)-N-(2-pyridinylmethylene)benzenamine (0.40 g, 1.5 mmol), and i-mu- chlorobis[(1,2,5,6- eta)-1,5-cyclooctadiene]diiridium (0.50 g, 1.0 mmol) were added to a solution of 1,3-dichloro-2-fluorobenzene (10.0 g, 60.6 mmol) in heptane (200 mL). The reaction mixture turned from yellow to forest green to brick red within the first minute. The reaction mixture was heated to reflux for 18 h. The mixture was then partitioned between ethyl acetate and water, and the aqueous extract was washed twice with ethyl acetate. The organic extracts were combined, dried over MgSOphi and concentrated under reduced pressure. The solid residue was purified by chromatography on silica gel by elution with ethyl acetate/hexane to afford the title compound as a solid (11.0 g). 1H NMR (CDCl3) delta 7.72 (d, 2H), 1.33 (s, 12H).

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, 2,6-Dichlorofluorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; E. I. DU PONT DE NEMOURS AND COMPANY; WO2009/51956; (2009); A2;,
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. 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride, A new synthetic method of this compound is introduced below., Product Details of 4584-46-7

To a stirred solution of 2-chloro-N,N- dimethylethan-1 -amine hydrochloride (2.00 g, 13.8 mmol) in DMF (20.0 ml_), at r.t under N2atmosphere, was added sodium azide (2.71 g, 41.7 mmol) portion wise over a period of 5 min. After complete addition the reaction mixture was heated at 60 C for 6 h. The reaction mixture was cooled to r. t and the contents were slowly poured onto water (50 ml.) and extracted with MTBE (2 x 100 ml_). The combined organic extracts were washed with brine (100 ml_), dried over anhydrous Na2S04, filtered and concentrated under vacuum to obtain 2-azido-N, N- dimethylethan-1 -amine.

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; THE SCRIPPS RESEARCH INSTITUTE; EXPANSION THERAPEUTICS, INC.; DISNEY, Matthew; BLIZZARD, Timothy, Allen; RZUCZEK, Suzanne; NDUNGU, John; VACCA, Joseph; JENNINGS, Andy; PUSHECHNIKOV, Alexei; (333 pag.)WO2019/99777; (2019); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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.

The synthesis of benzoaza-12-crown-4 is based on the condensation process of o-aminophenol with triethylene glycol dichloride in the presence of sodium hydroxide in the isopropanol medium. 17.4 g of o-aminophenol (0.16 mol) and 12.6 g of sodium hydroxide in 200 ml of isopropanol are placed into a flask, mechanically stirred, and kept at a temperature of 60 C for 60 min. After this 25 ml (0.16 mol) of triethylene glycol dichloride are dropped. The reaction mixture is kept boiling for 20 h. Then the mixture is cooled, acidified with hydrochloric acid to pH 3-4, filtered from inorganic impurities, alkalized with 25% ammonium hydroxide to pH 8-9, and evaporated on a rotary evaporator. The technical product obtained is distilled under vacuum and the high-boiling fraction is separated at a temperature of 150 C and pressure of 6 mm of mercury. The fraction is placed into a sealed vessel and kept at room temperature until the substance transition to the crystalline state. After crystallization the crystals are isolated, washed with acetone, and dried in the air. The product yield is 49 %.

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; Glushko; Sadovskaya; Blokhina; Anan’Ev; Journal of Structural Chemistry; vol. 56; 1; (2015); p. 142 – 147; Zh. Strukt. Kim.; vol. 56; 1; (2015); p. 149 – 154,6;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

70558-11-1, name is 6-Chloro-3,4-dihydro-2H-benzo[b][1,4]oxazine, belongs to chlorides-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: 6-Chloro-3,4-dihydro-2H-benzo[b][1,4]oxazine

Reference Example 82 Production of (6-chloro-2,3-dihydrobenzo[1,4]oxazin-4-yl)-(3,5-dibromo-4-hydroxyphenyl)-methanone 6-Chloro-3,4-dihydro-2H-benzo[1,4]oxazine (170.6 mg) obtained in Step 3 of Reference Example 51 and 3,5-dibromo-4-hydroxybenzoyl chloride (349.3 mg) obtained in Step 1 of Reference Example 4 were dissolved in ethyl acetate (5 mL), and the mixture was heated under reflux overnight. The solvent was evaporated, and the obtained solid was crystallized from methanol to give the title compound (441.0 mg) as crystals.

The synthetic route of 70558-11-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Japan Tobacco Inc.; US2008/305169; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 94-97-3, name is 5-Chloro-1H-benzo[d][1,2,3]triazole, 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. Formula: C6H4ClN3

a) A mixture of 5 g of 5-chlorobenzotriazole, 1.4 g of chloroacetone, 5.1 g of potassium carbonate and 0.5 g of potassium iodide is stirred into 50 mi of acetone at room temperature for 48 h. The mixture is subsequently filtered, the filtrate concentrated by evaporation in a vacuum, and the residue purified by flash chromatography. In this way, two isomeric products, [1- (5-CHLOROBENZOTRIAZOL-1-YI)-PROPAN-2-ONE] and [1-(6-CHLOROBENZOTRIAZOL-1-YL)-] propan-2-one, are isolated in approximately the same quantities, the first of which is then used directly in the next step.

The synthetic route of 5-Chloro-1H-benzo[d][1,2,3]triazole has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NOVARTIS AG; NOVARTIS PHARMA GMBH; WO2004/24704; (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. 6940-78-9, name is 1-Bromo-4-chlorobutane, A new synthetic method of this compound is introduced below., category: chlorides-buliding-blocks

Step 1 Synthesis of 1-(4-Chlorobutyl)-1,5,6,7-tetrahydroindol-4-one: To a solution of 1,5,6,7-tetrahydroindol-4-one (10.0 g, 74.0 mmol) in acetone (300 mL) was added powdered sodium hydroxide (3.26 g, 81.4 mmol) and the mixture stirred at ambient temperature for 0.25 h. 1-Bromo-4-chlorobutane (9.38 mL, 81.4 mmol) was then added and the resulting mixture stirred at ambient temperature for 7 h after which time TLC (ethyl acetate:dichloromethane 1:1) showed complete reaction. The reaction was gravity filtered to remove salts, and the filtrate concentrated to dryness under vacuum. The resulting residue was dissolved in dichloromethane (200 mL) and gravity filtered again to remove more salts. The filtrate was then washed with water, dried with sodium sulfate, filtered and the solvent removed under vacuum to yield an oil. Flash chromatography using 6 in. of silica gel in a 5.5 cm column eluding with 1:1 followed by 2:1 ethyl acetate:hexane on half of the residue yielded 9.0 g of an oil which contained ~6.0 g of pure product (72%) and ~3.0 g of acetone aldol condensation product (4-hydroxy-4-methyl-2-pentanone). The oil was taken to the next step without further purification.

The synthetic route of 6940-78-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Fick, David B.; Foreman, Mark M.; Glasky, Alvin J.; Helton, David R.; US2003/114463; (2003); 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. 94-97-3, name is 5-Chloro-1H-benzo[d][1,2,3]triazole, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 5-Chloro-1H-benzo[d][1,2,3]triazole

General procedure: in EtOAc/MeOH (4:1) mixture solvent (2 mL), benzotriazoles 1 (0.3 mmol), sodium sulfinates 2 (0.54 mmol), NaBr (0.36 mmol) and mCPBA (0.39 mmol) were added successively. The suspension mixture was vigorously stirred at room temperature for 4 h. Upon completion, the reaction was quenched by addition of sat. aq. Na2S2O3 (2 mL), basified with sat. aq. Na2CO3(8 mL) and H2O (5 mL). The mixture was extracted with CH2Cl2 (3×5 mL) and the combined organic phase was dried over anhydrous Na2SO4, filtered, and concentrated under reduced pressure. The residue was then purified by TLC technique (3:1 (v/v) petroleum ether/ethyl acetate) to furnish sulfonylbenzotriazoles 3.

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 94-97-3.

Reference:
Article; Wu, Sixue; Zhang, Yikun; Yan, Jie; Synthetic Communications; vol. 46; 17; (2016); p. 1432 – 1437;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 918538-05-3, 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. 918538-05-3, name is 2,4-Dichloropyrrolo[2,1-f][1,2,4]triazine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of 2,4-dichloropyrrolo[1,2-f][1,2,4]triazine (4a) (0.5 g, 2.7 mmol) in 2-Propanol (6 mL) was added (S)-pyrrolidin-2-ylmethanol (0.39 mL, 4.0 mmol), DIPEA (1.39 mL, 8.0 mmol) and heated at 90 C for 1 hr. The reaction was cooled to room temperature and solid obtained was collected by filtration to afford (S)-(l-(2-chloropyrrolo[2,l-f][l,2,4]triazin-4- yl)pyrrolidin-2-yl)methanol (96a) (0.49 g, 73 % yield) as a white solid; NMR (300 MHz, DMSO-i/e): delta 7.70 (dd, J= 2.6, 1.4 Hz, 1H), 6.97 (dd, J= 4.7, 1.6 Hz, 1H), 6.80 – 6.57 (m, 1H), 5.15 (t, J = 5.7 Hz, 1H, D2O exchangeable), 4.87 (t, J= 5.7 Hz, 1H), 4.44 (d, J= 17.8 Hz, 1H), 4.05 – 3.82 (m, 1H), 3.72 – 3.39 (m, 2H), 2.22 – 1.84 (m, 4H). MS (ES+): 253.3, 255.3 (M+2); MS (ES-): 287.2, 289.2 (M+Cl).

The synthetic route of 2,4-Dichloropyrrolo[2,1-f][1,2,4]triazine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BIOCRYST PHARMACEUTICALS, INC.; KOTIAN, Pravin, L.; BABU, Yarlagadda, S.; KUMAR, V., Satish; ZHANG, Weihe; LU, Peng-Cheng; RAMAN, Krishnan; (747 pag.)WO2018/232094; (2018); 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. 501-29-1, name is 1-Chloro-2-fluoro-4-methoxybenzene, This compound has unique chemical properties. The synthetic route is as follows., Formula: C7H6ClFO

To 1- chloro-2-fluoro-4-methoxybenzene (5.00 g, 31.2 mmol) in cone. H2SO4 (30 mL) at -10 C to 0 C, potassium nitrate (3.47 g, 34.4 mmol) was added portionwise to the reaction mixture. The reaction was stirred at 0 C for 2 h. The reaction was quenched with iced water and filtered. The obtained solids were recrystallized with hexanes to give Intermediate 15A (4.8 g, 75%).

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 501-29-1.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; THIBEAULT, Carl; CLARK, Charles, G.; DELUCCA, Indawati; HU, Carol, Hui; JEON, Yoon; LAM, Patrick, Y., S.; QIAO, Jennifer, X.; YANG, Wu; WANG, Yufeng; WANG, Tammy, C.; WO2014/22349; (2014); 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. 95-81-8, name is 2-Chloro-5-methylaniline, A new synthetic method of this compound is introduced below., category: chlorides-buliding-blocks

Example 1 Benzoyl chloride (21.9 g) was added dropwise to a stirred mixture of ammonium thiocyanate (13.2 g) in acetone (95 ml) and the mixture stirred for a further 20 minutes at room temperature. A solution of 6-chloro-m-toluidine (22.1 g) in acetone (30 ml) was added dropwise with stirring, the mixture stirred for a further 30 minutes at room temperature and then heated under reflux for 5 minutes. The mixture was added to water, the solid collected, dissolved in aqueous sodium hydroxide (10%; 95 ml) acidified to pH 5 with hydrochloric acid and rebasified to pH 9 with aqueous ammonia. The solid was filtered and recrystallized from toluene to give 1-(6-chloro-m-tolyl)thiourea, m.p. 152-4.

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; SCHERING AGROCHEMICALS LIMITED; EP337616; (1989); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics