Tag: M.W=200-300

Related Products of 1435-50-3, 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 1435-50-3 as follows.

Reference Example 76 1-(2,5-dichlorophenyl)-6-methoxyindan-1-ol To a solution of 1-bromo-2,5-dichlorobenzene (4.18 g, 18.5 mmol) in THF (25 mL) was added dropwise 1.6 M n-butyllithium hexane solution (13.8 mL, 22.1 mmol) at -78C, and the mixture was stirred for 30 min. Then, a solution of 6-methoxyindan-1-one (2.00 g, 12.3 mmol) in THF (15 mL) was added dropwise, and the mixture was stirred for 1 hr. To the reaction mixture was added saturated aqueous ammonium chloride solution and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to give the title compound (1.95 g, yield 51%) as an oil. 1H-NMR (CDCl3) delta: 2.29 – 2.42 (1H, m), 2.52 (1H, s), 2.79 – 3.00 (2H, m), 3.04 – 3.23 (1H, m), 3.73 (3H, s), 6.53 (1H, d, J = 2.4 Hz), 6.87 (1H, dd, J = 8.3, 2.4 Hz), 7.16 – 7.30 (3H, m), 7.70 (1H, d, J = 2.3 Hz).

According to the analysis of related databases, 1435-50-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Takeda Pharmaceutical Company Limited; EP2298731; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 14862-52-3, 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. 14862-52-3 name is 3,5-Dibromochlorobenzene, 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.

Preparation of compound 7-1 After dissolving 1,3-dibromo-5-chlorobenzene (20 g, 73.98 mmol), phenyl boronic acid (22 g, 177.55 mmol), and Pd(PPh3)4(4.3 g, 3.699 mmol) in a mixture solvent of 2 M K3PO4aqueous solution 100 mL, toluene 400 mL, and 1,4-dioxane 100 mL in a flask, the mixture was stirred under reflux at 120C for 5 hours. After completing the reaction, an organic layer was extracted with ethyl acetate, and the remaining moisture was removed using magnesium sulfate. The residue was dried and separated with column chromatography to obtain compound 7-1 (23 g, 70%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3,5-Dibromochlorobenzene, and friends who are interested can also refer to it.

Reference:
Patent; ROHM AND HAAS ELECTRONIC MATERIALS KOREA LTD.; KANG, Hee-Ryong; KANG, Hyun-Ju; HONG, Jin-Ri; MOON, Doo-Hyeon; LIM, Young-Mook; KIM, Bitnari; KIM, Nam-Kyun; WO2015/178731; (2015); 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. 19752-55-7, name is 1-Bromo-3,5-dichlorobenzene, A new synthetic method of this compound is introduced below., HPLC of Formula: C6H3BrCl2

Example 2; Step 1; Magnesium turnings (5.38 g) and THF (50 ml) were placed in a dry flask equipped with a dropping funnel which contained a mixture of 1-bromo-3,5-dichiorobenzene (50 g) and THF (300 ml). 30 Milliliters of the solution in the dropping funnel was added to the flask. A few drops of dibromoethane were added to he flask to help initiate the reaction. After a few minutes, solvent in the reaction flask started to boil. The remaining solution in the dropping funnel was added drop wise. Ice water was used occasionally to coo. the reaction mixture. After the addition, the mixture was stirred at room temperature for two hours. Benzonitriie (22,82 g) was added to the reaction mixture. The mixture was refiuxed for 2 days. 3 N HC1 (300 mL} was added, The mixture was stirred for 4 hours and extracted using ethyl acetate. The organic layer was collected in a separatory funnel and concentrated. The obtained oil (49 g) was used in the next step without further purification.

The synthetic route of 19752-55-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TRANSITIONS OPTICAL, INC.; WO2012/82506; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

69695-61-0, name is 2-Chloro-4-(trifluoromethoxy)aniline, 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: 2-Chloro-4-(trifluoromethoxy)aniline

a) 2-Chloro-4-trifluoromethoxybenzenesulfonyl chloride 2-Chloro-4-trifluoromethoxyaniline is reacted to give the corresponding sulfonyl chloride by the same protocol as in Example 6a).

The synthetic route of 69695-61-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SANOFI-AVENTIS DEUTSCHLAND GMBH; US2007/197539; (2007); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 51419-59-1, These common heterocyclic compound, 51419-59-1, name is p-Tolylmethanesulfonyl chloride, 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.

General procedure: 5-Chloro-2-nitroaniline (173 mg, 1 mmol) was dissolved in DMF (3 mL) and dry sodium hydride (120 mg, 5 mmol) was added.The obtained mixture was stirred for 1 min and the suitable substitutedbenzenesulfonyl chloride 1 (a?g) or phenylethanesulfonylchloride 3 (a?g) (1,5 mmol) was added in several portions. The reaction was quenched after 2?6 h through the addition of a saturated NaHCO3 aqueous solution (5 mL). The mixture was extractedwith EtOAc (3 10 mL) and dried over Na2SO4. After removal ofthe solvent under reduced pressure, the residue was purified byflash chromatography using cyclohexane/AcOEt (80:20) as eluentand crystallized from Et2O.

The synthetic route of 51419-59-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Ferro, Stefania; Buemi, Maria Rosa; De Luca, Laura; Agharbaoui, Fatima E.; Pannecouque, Christophe; Monforte, Anna-Maria; Bioorganic and Medicinal Chemistry; vol. 25; 14; (2017); p. 3861 – 3870;,
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. 202197-26-0, name is 3-Chloro-4-((3-fluorobenzyl)oxy)aniline, A new synthetic method of this compound is introduced below., COA of Formula: C13H11ClFNO

General procedure: Acetic acid (2.0 mL) and aniline derivatives (1.10mmol) was added to 6 (1.00 mmol). The mixturewas heated to 125-130 C andstirred for 15 min. The reaction mixture was then cooled to 25 C.The acetic acid was evaporated. To the reaction mixture, ice-water(10 mL) was added and adjusted pH to 9 with ammonium hydroxide.The mixture was stirred for 0.5 h. The precipitated productwas filtered, and the filtered cake was washed with water(3 x 10 mL) to afford crude product. The crude product was chromatographedby silica gel, eluting with EtOAc/petroleum ether(1:4) to afford 7a-7f (yield 82-94%) as white solid. 4.1.7.1 4-(3-chloro-4-(3-fluorobenzyloxy)phenylamino)-6,7-bis(2-chloroethoxy)quinazoline (7a) Yield: 86%. 1H NMR (600?MHz, DMSO-d6) delta(ppm): 9.47 (s, 1H), 8.48 (s, 1H), 7.97 (d, J?=?2.6?Hz, 1H), 7.91 (s, 1H), 7.71 (dd, J?=?8.9, 2.6?Hz, 1H), 7.50-7.46 (m, 1H), 7.35-7.31 (m, 2H), 7.28 (s, 1H), 7.26 (s, 1H), 7.20-7.16 (m, 1H), 5.25 (s, 2H), 4.48-4.45 (m, 4H), 4.08 (t, J?=?5.5?Hz, 2H), 4.04 (t, J?=?5.0?Hz, 2H). 13C NMR (151?MHz, DMSO-d6) delta(ppm): 162.2 (d, 1JC-F?=?243.7?Hz), 156.3, 153.2, 153.1, 149.5, 147.5, 147.0, 139.7, 139.6, 133.4, 130.5 (d, 3JC-F?=?8.3?Hz), 124.0, 123.3 (d, 4JC-F?=?2.6?Hz), 122.1, 121.1, 114.6 (d, 2JC-F?=?20.9?Hz), 114.3, 114.0 (d, 2JC-F?=?21.9?Hz), 109.0 (d, 3JC-F?=?8.6?Hz), 104.7, 69.5, 69.4, 68.9, 42.7, 42.6.

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, Yaling; Chen, Li; Xu, Hongjiang; Li, Xiabing; Zhao, Lijun; Wang, Wei; Li, Baolin; Zhang, Xiquan; European Journal of Medicinal Chemistry; vol. 147; (2018); p. 77 – 89;,
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. 38762-41-3, name is 4-Bromo-2-chloroaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of 4-Bromo-2-chloroaniline

General procedure: Phenyl phenylphosphoramidochloridate (1) (0.001 mol) and 2-amino-benzothiazole (2a) (0.001 mol) were taken in a bottomed flask (50 mL) and THF (20 mL) was added. To thismixture, dimethylpiperazine (DMP) (0.001 mol) was added andthe reaction mixture was stirred vigorously at 30-50 C for 4 h.The progress of the reaction was monitored by TLC. After completionof the reaction, DMP. HCl was removed by filtration andthe filtrate was concentrated under vacuum and the resultantsolidwas purified by passing through a columnof silica gel usinghexane:ethyl acetate (2:1) as an eluent to afford title compound,phenylN-1,3-benzothiazol-2-yl-N?-phenylphosphorodiamidate(3a). The same experimental procedure was adopted for the preparation of the remaining title compounds (3b-j) (Scheme 1).

The synthetic route of 38762-41-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Nayab Rasool; Babu, P. Hari; Janaki Ramudu; Jyothi Kumar; Appa Rao, Ch.; Raju, C. Naga; Phosphorus, Sulfur and Silicon and the Related Elements; vol. 193; 1; (2018); p. 10 – 13;,
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. 19752-55-7, name is 1-Bromo-3,5-dichlorobenzene, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 19752-55-7

To a solution of 1-bromo-3,5-dichlorobenzene (25.0 g, 1 10.6 mmol) in 400 ml THF at room temperature, isopropyl magnesium chloride lithium chloride complex (85.0 ml, 1.3M THF, 1 10.6 mmol) was added dropwise at room temperature over a period of 15 minutes while holding the reaction temperature between 20°C and 25°C. After the addition was complete, the reaction was allowed to stir 1.5 hours at room temperature. The reaction solution was then cooled to -5 °C to -10 °C with ice/MeOH. Methyltrifluoroacetate (12.23 ml, 121 .6 mmol) in 20 ml THF was added dropwise to the reaction solution while maintaining the reaction temp below 0 °C (~ 30 min). The reaction was stirred at -5 °C for 0.5 hr then was allowed to warm to room temperature and stir for 1.5 hrs. The reaction was cooled again to -5 °C to -10 °C then 73.7 ml 6M HCI diluted to 150 ml total volume water was added dropwise while keeping the temperature below 0 °C. Once the addition was complete, the reaction was stirred 0.5 hr at 0 °C then was allowed to warm to room temperature. Excess water was added and the resulting organic layer that separated was drawn off. The aqueous layer was washed repeatedly with DCM. The combined DCM washes and recovered organic layer were dried over sodium sulfate and concentrated to yield 90 g of an oil. The crude material was then passed through a silica gel plug (neat heptane to neat DCM) and purified by vacuum distillation (3 torr, product fractions recovered froml 12 °C to 125 °C) to provide 20.3 g product (75.7percent yield). 1 H NMR (400 MHz, CHLOROFORM-d) delta ppm 7.71 (s, 1 H) 7.93 (s, 2 H). IR 1728.1 cm”1

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 19752-55-7.

Reference:
Patent; AVISTA PHARMA SOLUTIONS, INC.; SPEAKE, Jason, D.; (57 pag.)WO2018/9751; (2018); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 201849-21-0,Some common heterocyclic compound, 201849-21-0, name is 4-Bromo-2-chloro-1-isopropoxybenzene, molecular formula is C9H10BrClO, 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.

A mixture of Compound 27B (1.35 g, 5.4mmol), Pd(dppf)C12 (0.35 g, 0.43 mmol), 4,4,4,4,5,5,5?, 5?-octamethyl-2,2?-bi( 1,3 ,2-dioxaborolane) (2.09 g, 8.22 mmol), and potassium acetate (1.62 g, 16.5 mmol) in 1,4-dioxane (50 ml) was heated at 80C for 16 hours. The mixture was diluted with water (200 mL) and extracted with ethyl acetate (200 mL x 2). The combined extracts were washed with water (200 mL) and brine (200 mL), dried over anhydrous sodium sulfate, filtered, and concentrated. The residue was purified with flash column chromatography on silica gel (ethyl acetate in petroleum ether, from 0% to 10% v/v) to furnish Compound 27C. LC-MS (ESI) m/z: non-ionizable compound under routine conditions used.

The synthetic route of 201849-21-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BIOMARIN PHARMACEUTICAL INC.; WANG, Bing; CHAO, Qi; (737 pag.)WO2019/133770; (2019); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 1996-30-1, 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. 1996-30-1, name is 3-Bromo-4-fluorochlorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To an oven-dried 25 mL Schlenk tube containing a stirring bar was added 4.5 mg Pd(OAc)2 (0.02 mmol), 15.7mg nBuPAd2 (0.44 mmol), 2-bromofluorobenzene (0.50 mmol), salicylaldehyde (0.50 mmol), potassium carbonate (1.0 mmol). The Schlenk tube was vacuumed and then purged with argon before DMF (2.0 mL) was injected using a syringe. Afterwards the Schlenk tube in the ice bath was degassed by evacuation and back fillingwith argon three times. The reaction mixture was then stirred for 12 h at 120 C. After the reaction was complete,the reaction mixture was diluted with water (5 mL), extracted with ethyl acetate (3 x 10 mL) and dried withanhydrous Na2SO4. After filtration and addition of silica gel into the solution, the organic solvent was reduced evaporated. The crude product was purified by column chromatography using ethyl acetate/n-pentane.

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-Bromo-4-fluorochlorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Shen, Chaoren; Wu, Xiao-Feng; Synlett; vol. 27; 8; (2016); p. 1269 – 1273;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics