Chlorides-buliding-blocks

These common heterocyclic compound, 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, 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. SDS of cas: 2533-69-9

Step 1-Synthesis of 4-[6-bromo-2-(trichloromethyl)-1,3-benzodiazol-1-yl]pyrimidin-2-amine To a solution of 4-N-(2-amino-5-bromophenyl)pyrimidine-2,4-diamine (3.0 g, 10.71 mmol) in acetic acid (10 mL) was added methyl 2,2,2-trichloroethanimidoate (1.4 mL, 11.25 mmol). The reaction was stirred at 45 C. for 7 hr. Water (15 mL) was then added. The precipitate was collected by filtration and dried under vacuum to give the title product (3.94 g as the acetic acid salt); 1H NMR (500 MHz, DMSO) delta 1.90 (3H, s), 7.01 (1H, d, J=5.0 Hz), 7.21 (2H, s), 7.75-7.46 (2H, m), 8.09-7.75 (1H, m), 8.58 (1H, d, J=5.0 Hz); LC-MS: m/z=+406/408/410/412 (M+H)+.

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

Reference:
Patent; Genentech, Inc.; US2012/214762; (2012); 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. 622-86-6, name is (2-Chloroethoxy)benzene, A new synthetic method of this compound is introduced below., SDS of cas: 622-86-6

Example 29 N-2-(4-(2-phenoxyethoxy)-phenyl)-propyl-2-propanesulfonamide. To a stirred mixture of N-tertbutoxyacetyl-2-(4-hydroxyphenyl)propyl-2-propanesulfonamide (0.250 g,.70 mmol) in dry dimethylformamide (4 mL) was added sodium hydride (0.062 g, 0.87 mmol) under nitrogen. The resulting mixture was stirred 30 minutes at ambient temperature or until hydrogen gas evolution had ceased. Next, beta-chlorophenetole (0.120 g, 0.77 mmol) and sodium iodide (0.042 g, 0.25 mmol) are added and the resulting mixture was heated to 65C for 12 h. The resulting mixture was cooled and partitioned between ethyl acetate and water. The organic layer was washed with water (2 X 20 mL) and brine (1 X 20 mL), dried over magnesium sulfate, and filtered. Evaporation of the filtrate in vacuo followed by chromatography on silica gel eluding with ethyl acetate-hexane gave 0.250 g (75%) of the protected sulfonamide. To a stirred mixture of dichloromethane: trifluoroacetic acid (2 mL, 1:1) was added the protected sulfonamde (0.220 g, 0.42 mmol) under nitrogen. The resulting mixture was stirred at ambient temperature for 4 h. The mixture was partitioned between dichloromethane and 10% aqueous potassium carbonate. The organic layer was washed with brine (1 X 20 mL), dried over magnesium sulfate, and filtered. Evaporation of the filtrate in vacuo gives 0.166 g (96%) of the pure title compound. Mass Spectrum: MS +1= 378.5

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; ELI LILLY AND COMPANY; EP994110; (2000); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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 4584-46-7 as follows. Application In Synthesis of 2-Chloro-N,N-dimethylethanamine hydrochloride

Caesium carbonate (3.0 Eq), sodium iodide (0.14 Eq) and 2-chloro-N,N- dimethylethylamine hydrochloride (1.5 Eq) are added to a suspension of p-bromo-phenol (1.0 Eq) in butanone (50 mL). The suspension is kept under reflux for four hours, after which the solid is filtered through a Hirsch funnel and washed with acetone, and the solvent is evaporated at low pressure. The crude product (yellow oil) is purified by silica-gel chromatography (eluent: dichloromethane-methanol; 95:5) to obtain the desired product (2-p-bromophenoxyethyl-N,N-dimethylamine) as a colourless oil (yield 70%).

According to the analysis of related databases, 4584-46-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; UNIVERSITA’ DEGLI STUDI DI MILANO; FUMAGALLI, Laura; PICOZZI, Claudia; REGAZZONI, Luca; CARINI, Marina; ALDINI, Giancarlo; VISTOLI, Giulio; (26 pag.)WO2019/53626; (2019); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 1005-56-7,Some common heterocyclic compound, 1005-56-7, name is O-Phenyl carbonochloridothioate, molecular formula is C7H5ClOS, 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 alcohol 12 (150 mg, 0.288 mmol), pyridine (93 muL, 1.15 mmol) and DMAP (3.5 mg, 29 mumol) in dry CH2Cl2 (28 mL) was added phenyl chlorothionoformate (80 muL, 0.576 mmol) at room temperature. After being stirred at 40 C for 2.5 h, the reaction mixture was poured into H2O (60 mL). The mixture was extracted with AcOEt (50 mL x3). The combined organic layer was washed with brine (100 mL), and dried over anhydrous Na2SO4. The solution was concentrated to dryness in vacuo. The residue was purified by flash column chromatography (silica gel 4 g, AcOEt/hexane 1:9?1:4) to give phenyl thiocarbonate S1 (178 mg, 94%) as a white solid.

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

Reference:
Article; Adachi, Masaatsu; Sakakibara, Ryo; Satake, Yoshiki; Isobe, Minoru; Nishikawa, Toshio; Chemistry Letters; vol. 43; 11; (2014); p. 1719 – 1721;,
Chloride – Wikipedia,
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Synthetic Route of 622-86-6, 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 622-86-6 as follows.

5.23mL of 1-(2-chloroethoxy)benzene (38.45mmol), previously distilled on CaH2, were dissolved in 50mL of dry THF to give a colorless solution. 25mL of a solution 2M of sodium cyclopentadienide in THF were added drop-wise at -78C. The solution was warmed up to room temperature and left stirred overnight to give a white precipitate and a dark pink solution. Afterwards the mixture was quenched with methanol and cold water. The organic product was extracted by 3x 50mL ether fraction. The solution was dried over magnesium sulphate and had its solvent removed at reduced pressure to yield a brown oil (yield 89%). 1H NMR (300MHz, CDCl3) delta 2.88 [t, 2H, C5H5-(CH2CH2OC6H5),], 4.14 [t, 2H, C5H5-(CH2CH2OC6H5)], 3.01-3.20 [m, 1H, C5H5-(CH2CH2OC6H5)], 6.17-6.52 [m, 4H, C5H5-(CH2CH2OC6H5)], 6.92-7.32 [m, 5H, C5H5-(CH2CH2OC6H5)]. 13C NMR (75MHz, C6D6) delta 30.1 [C5H5-(CH2CH2OPh)], 67.8 [C5H5-(CH2CH2OPh)], 44.1 [C5H5-(CH2CH2OPh)], 114.8, 120.9, 128.1, 129.7, 134.4, 134.9, 159.1 [C5H5-(CH2CH2OPh)]. Mass (GC-MS): 186.1 [M]+.

According to the analysis of related databases, 622-86-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Saturnino, Carmela; Sirignano, Esther; Botta, Antonio; Sinicropi, Maria Stefania; Caruso, Anna; Pisano, Assunta; Lappano, Rosamaria; Maggiolini, Marcello; Longo, Pasquale; Bioorganic and Medicinal Chemistry Letters; vol. 24; 1; (2014); p. 136 – 140;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 873-38-1, name is 2-Bromo-4-chloroaniline, 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 873-38-1, category: chlorides-buliding-blocks

Step 1: 2-Bromo-4-chloroaniline (1.0 eq) was dissolved in CH2Cl2 (0.25 M), then triethylamine and trifluoroacetyl anhydride (1.1 eq each) were added. The resulting mixture was stirred at room temperature for 1 hour. The solvent was evaporated and the residue was purified by flash chromatography with CH2Cl2 as eluent to give the amide in 97% yield. m/z(M-H)- 300.0

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; ZIARCO PHARMA LIMITED; LIU, Wai Leung; PURKINS, Lynn; YEADON, Michael; (23 pag.)US2017/7576; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 14862-52-3, 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. 14862-52-3, name is 3,5-Dibromochlorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 3 General Procedure C To the aryl halide (2.0 mmol), Pd2(dba)3 (37 mg, 0.04 mmol, 2 mol %) and 2-(dicyclohexylphosphino)biphenyl (34 mg, 0.1 mmol, 4.8 mol %) were added LiHMDS (803 mg, 4.8 mmol, 2.4 equiv.) and 4 mL toluene. The reaction mixture was stirred at room temperature for 17 h. At reaction completion, the mixture was quenched with 1N HCl (5 mL) and stirred at room temperature for 5 min. Then, it was basified to pH=12 with 1N NaOH and the layers were separated. The organic layer was concentrated. 5-Chlorobenzene-1,3-diamine General Procedure C was followed using 5-chloro-1,3-dibromobenzene (540 mg, 2.0 mmol). The product was isolated as a brown oil in 97% yield (299 mg, 105% mass recovery and 83% purity). 1H NMR (400 MHz, CDCl3): delta 6.10 (s, 2 H), 5.87 (s, 1 H), 3.60 (br s, 4 H); 13C NMR (100 MHz, CDCl3): delta 148.3, 135.5, 105.9, 99.7; HRMS calcd for C6H8N2Cl (M+H) 143.0370, found 143.0369.

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, 3,5-Dibromochlorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Boehringer Ingelheim International, GmbH; US2006/258888; (2006); 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. 56961-77-4, name is 1-Bromo-2,3-dichlorobenzene, A new synthetic method of this compound is introduced below., Quality Control of 1-Bromo-2,3-dichlorobenzene

Intermediate 45:[0178] To a -30C solution of l-bromo-2,3-dichlorobenzene (10 g, 44 mmol) in THF (120 mL) was added z-PrMgCl (2.0 M in THF, 35 mL, 70 mmol) at a rate such that the temperature < -20C. Meanwhile, to a -10C solution of Cul (420 mg, 2.2 mmol) in THF (120 mL) was added pyridine (7.1 mL, 88 mmol) and then benzyl carbonochloridate (9.7 mL, 68 mmol) such that the temperature < 0C. To this heterogeneous mixture was added the initially formed Grignard at a rate such that the temperature < 0C. The resulting solution was stirred at 0C for 30 min and then allowed to warm to rt. The reaction was then quenched with 10% aq NH4C1. EtOAc was added and the blue aq layer was removed. The organic layer was washed with 10% aq H4CI, 1 N HC1, and a 20% aq NaCl solution. The organic layer was then concentrated and the residue was dissolved and crystallized from MeOH. The slurry was filtered and the filtercake washed with MeOH to give benzyl 4-(2,3-dichlorophenyl)pyridine-l(4H)- carboxylate (intermediate 45) (12 g, 76%) as an off-white solid. HPLC: 99%, RT 4.118 min. MS (ESI) m/z 382.0 [M + Na]+. mp: 69-70C. 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 UNIVERSITY OF NORTH CAROLINA AT CHAPEL HILL; JIN, Jian; ROTH, Bryan; FRYE, Stephen; WO2012/3418; (2012); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 6579-54-0, 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 6579-54-0 as follows.

General procedure: To a stirred solution of 4 (1.0 mmol) in THF (5 mL) was added appropriate sulfonyl chloride (1.1 mmol) and NaHCO3 (38 mmol). The reaction mixture was stirred at room temperature for 4 h under nitrogen atmosphere. Then the solvent was evaporated in vacuum. The residue was diluted with water. The whole mixture was extracted with AcOEt for three times. The combined organic layer was washed with water, sat. brine, and dried over Na2SO4. The crude product was purified by column chromatography using petroleum ether/AcOEt (10/1-8/1, v/v) as eluent to afford F01-F35.

According to the analysis of related databases, 6579-54-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Zhang, Wen-Ming; Yao, Yang; Yang, Teng; Wang, Xue-Ying; Zhu, Zhen-Yun; Xu, Wen-Tao; Lin, Hai-Xia; Gao, Zhao-Bing; Zhou, Hu; Yang, Cai-Guang; Cui, Yong-Mei; Bioorganic and Medicinal Chemistry Letters; vol. 28; 10; (2018); p. 1943 – 1948;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 27139-97-5, 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. 27139-97-5, name is 2-Bromo-4-chloro-1-methylbenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

(b) 50 g of compound 3, 50 g of NBS (ie N-bromosuccinimide), 0.3 g of BPO (ie dibenzoyl peroxide) and 300 mL of carbon tetrachloride were added to a 500 mL three-necked flask, and the external temperature was raised to At 90 C, the reaction was carried out for 24 h (at this time, TLC showed complete reaction);Pour the reaction solution into 500 mL of ice water, adjust the pH to 10 with 2N (equivalent concentration) sodium hydroxide solution, extract the layers, combine the organic phases, and wash with 5% sodium bicarbonate (mass concentration, the same below) solution. After drying, it was spin-dried, and column chromatography was carried out to obtain 52 g of Compound 4 (yield: 75%) (the nuclear magnetic spectrum of Compound 4 is shown in Fig. 3, and the specific resolution is: 1H NMR (400 MHz, CDCl3) delta (ppm): 7.58 ( d, J = 2.0 Hz, 1H), 7.38 (d, J = 4.0 Hz, 1H), 7.28 (d, J = 4.0 Hz, 1H), 4.55 (s, 1H))

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-Bromo-4-chloro-1-methylbenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Liu Ke; (11 pag.)CN108707112; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics