Tag: M.W=200-300

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. 50638-46-5, name is 4-Bromo-3-chloroanisole, A new synthetic method of this compound is introduced below., Safety of 4-Bromo-3-chloroanisole

A 1.6M solution of n-butyllithium in hexane (4 ml) was added to a solution of 4-bromo-3-chloroanisole (CAS Reg. No. 50638-46-5, 1.3 g) in THF (20 ml) at -78 C. The mixture was stirred for 30 min at -78 C. Acetaldehyde (0.7 ml) was added to the mixture. The mixture was allowed to warm to room temperature. Water (50 ml) was added and extracted with DCM. The combined organic layers were dried over Na2SO4 and concentrated to an oil to give the title compound (983 mg) as colorless oil. MS (m/e)=186 [M+].

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; Hunziker, Daniel; Lerner, Christian; Mueller, Werner; Sander, Ulrike Obst; Pflieger, Philippe; Waldmeier, Pius; US2010/249124; (2010); 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. 60811-21-4, name is 4-Bromo-2-chloro-1-fluorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 4-Bromo-2-chloro-1-fluorobenzene

Step 1. Preparation of 6-bromo-2-chloro-3-fluorobenzaldehyde (i-9b) [00169] To a solution of 4-bromo-2-chloro-l-fluorobenzene (5.00 g, 23.9 mmol) in THF (40 mL) was added lithium diisopropylamide (14.3 mL, 28.6 mmol) dropwise at -78 C. The resultant mixture was stirred at -78 C for 2 h and then DMF (2.70 mL, 35.8 mmol) was added. The reaction mixture was warmed to room temperature, quenched with aq. NH4C1, and extracted with EtOAc (3×100 mL). The combined organic layers were concentrated and purified by chromatography (0-10% EtOAc in petroleum ether) to give the title compound. XH NMR (400 MHz, CDC13) delta 10.27-10.33 (m, 1H), 7.56 (dd, J = 8.6 Hz, 4.3 Hz, 1H), 7.18-7.26 (m, 1H).

The synthetic route of 60811-21-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK SHARP & DOHME CORP.; LAPOINTE, Blair, T.; FULLER, Peter, H.; GUNAYDIN, Hakan; LIU, Kun; SCOTT, Mark, E.; TROTTER, B., Wesley; ZHANG, Hongjun; (211 pag.)WO2017/75182; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 309721-44-6, The chemical industry reduces the impact on the environment during synthesis 309721-44-6, name is 2-Bromo-1-chloro-3-fluorobenzene, I believe this compound will play a more active role in future production and life.

General procedure: A 250 mLround-bottom flask was charged with 1-bromo-4-chloro-2-fluoro-benzene (8.5 mL,68.0 mmol), hydrazine monohydrate (13 mL, 270 mmol) and dimethylsulfoxide (25mL) and the solution was stirred at 70 C for 3 days. The reaction was thencooled to room temperature and water (200 mL) was added. The precipitate was collected by filtration and dried under vacuum for 16 hours

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-1-chloro-3-fluorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Rene, Olivier; Fauber, Benjamin P.; Tetrahedron Letters; vol. 55; 4; (2014); p. 830 – 833;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 53531-69-4, name is (4-Bromophenyl)methanesulfonyl chloride, 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 53531-69-4, Product Details of 53531-69-4

C-(4-Bromophenyl)-N-(2,4-dimethoxybenzyl)methanesulfonamide While cooling with ice, 20.0 g of 4-bromobenzylsulfonyl chloride were initially charged in 200 ml of dichloromethane, and a solution of 24 ml of 2,4-dimethoxybenzylamine in 100 ml of dichloromethane was slowly added dropwise. For improved stirrability, a further 100 ml of dichloromethane were added, and the reaction mixture was allowed to come to room temperature. After stirring for 2 hours, the reaction mixture was washed with 100 ml of water, with 100 ml of 0.2 N aqueous hydrochloric acid, with 100 ml of saturated aqueous sodium hydrogencarbonate solution and finally once more with 100 ml of water. The organic phase was dried over Na2SO4, concentrated by rotary evaporation and dried under high vacuum. The residue (30 g) was used in the next reaction without further purification.

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, (4-Bromophenyl)methanesulfonyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SANOFI; Boehme, Thomas; Ritter, Kurt; Engel, Christian; Haack, Torsten; Guessregen, Stefan; Tschank, Georg; US2013/345127; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 89794-02-5, 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. 89794-02-5 name is 4-Bromo-2-chlorotoluene, 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.

10.0 mmol of the specified boronic ester (I; R1), 30.0 mmol of magnesium turnings and 5.0 mmol of the salt (II) are suspended in a mixture of 3.40 g of anhydrous toluene and 0.73 g of anhydrous tetrahydrofuran in a dry four-neck flask under a nitrogen atmosphere with a mechanical stirrer, thermometer, metal condenser and pressure-equalized dropping funnel, and stirred vigorously for 30 min. The appropriate haloaromatic (III, R4) is added to this solution, at first in undiluted form, until the onset of exothermicity signals the start of the reaction. The remaining total amount of 30.6 mmol of haloaromatic is diluted with 10.0 g of anhydrous toluene and 10.0 g of anhydrous tetrahydrofuran and added dropwise at such a rate that the internal temperature does not exceed 45 C. On completion of addition, the reaction mixture is heated at reflux for 1 h or until the dissolution of the magnesium was complete. The resulting suspension is discharged onto 50 g of ice-water, and the resulting solids are isolated, washed with cold water and dried under reduced pressure. The composition of Examples 77-91 and selected physical properties are summarized in Table 3.

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

Reference:
Patent; Covestro Deutschland AG; ROeLLE, Thomas; BERNETH, Horst; HOeNEL, Dennis; BRUDER, Friedrich-Karl; (34 pag.)US2019/276479; (2019); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 98577-44-7, name is 1,1-Dibromo-2,2-bis(chloromethyl)cyclopropane, 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 98577-44-7, Quality Control of 1,1-Dibromo-2,2-bis(chloromethyl)cyclopropane

(1) Equipment specifications: three-stage 1000mL CSTR reactor (continuous stirring tank reactor, full mixed anaerobic reactor), 50ml plunger pump, 5000g balance, 1.0L feeding bottle. (2) Proportion of raw materials: Solution A: 5.0 kg of 1,1-dibromo-2,2-chloromethylcyclopropane + 2.0 vol n-butyl ether, L1 (feed rate of solution A) = 4.5 g / min; Solution B: 2.2eq lithium phenyl / n-butyl ether solution, L2 (feed rate of solution B) = 4.5g / min; Solution C: 1.0 g / g ammonia; L3 (feed rate of solution C) = 1.0 g / min. (3) Reaction conditions: three-stage CSTR, the first-stage low-temperature section is controlled at -50 to 0 C, and the retention volume is 500ml; the second and third-stage reaction sections are controlled at 0 C, the retention volume is 700ml, and the third-stage overflow To the receiving bottle, the temperature of the receiving bottle was controlled at 0 C, the total retention volume was 1200 ml, and the RT (retention time) = 2.0 h. Turn on the automatic feeding system, two feeds, L1 = 4.5g / min, L2 = 4.5g / min, the two feeds are mixed through the low-temperature section of the first-stage CSTR, and after 40 minutes, overflow to the second- and third-stage reaction sections After 70 minutes of reaction, the third-stage CSTR began to overflow to the receiving bottle, and the charging system was started. L3 = 1.0 g / min, and the reaction was quenched by continuous injection of ammonia water. Post-treatment, liquid separation, and low-temperature distillation gave 0.761 kg (converted content) of the product, and the NMR yield was 68%.

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

Reference:
Patent; Jilinkai Laiying Pharmaceutical And Chemical Co., Ltd.; Hong Hao; Zhang Enxuan; Lu Jiangping; Wei Fuliang; Yang Sihang; (11 pag.)CN110117215; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 73006-78-7, 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. 73006-78-7, name is 5-Chloro-[1,1′-biphenyl]-2-amine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

250 mL under a stream of nitrogenCompound 2-A (6.0 g, 29.46 mmol) in flask,1-naphthalene boronic acid (6.08 g, 35.35 mmol),Potassium triphosphate (15.63 g, 73.65 mmol),Palladium (II) acetate (0.198 g, 0.884 mmol),2-dicyclohexylphosphino-2 ‘, 6′-dimethoxybiphenyl (0.726 g, 1.767 mmol), toluene (100 mL) and H2O (10 mL) were added thereto, and the mixture was stirred and refluxed.After completion of the reaction, the toluene layer was extracted using toluene and water. The extracted solution was treated with MgSO 4 to remove residual water, concentrated under reduced pressure, and purified by column chromatography to give a compound 2-B.6.16 g was obtained in 70.8% yield.

The synthetic route of 5-Chloro-[1,1’-biphenyl]-2-amine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Material Science Co.,Ltd.; Lee Tae-wan; Huh Jeong-hoe; Lee Dong-hun; Park Seong-min; Kim Seon-jae; Kim Seong-hun; (44 pag.)KR102041137; (2019); 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. 6579-54-0, name is 2,6-Dichlorobenzenesulfonyl chloride, A new synthetic method of this compound is introduced below., name: 2,6-Dichlorobenzenesulfonyl chloride

Example 14 N-[(5-Isobutyl-1-phenyl-1H-pyrazol-3-yl)methyl]-2,6-dichlorobenzenesulfonamide (Compound 14) To a solution of (5-isobutyl-3-aminomethyl-1-phenyl)pyrazole (42.6 mg, 0.186 mmol) in dichloromethane (2.0 mL) was added triethylamine (28.5 muL, 0.204 mmol) at 0 C. The solution was stirred for 5 min, and mixed with a solution of 2,6-dichlorobenzenesulfonyl chloride (48.3 mg, 0.195 mmol) in dichloromethane. Subsequently, the solution was warmed to room temperature, and stirred for 1 hr. Then, water and a saturated sodium hydrogen carbonate solution were added to the solution before extraction with dichloromethane. The organic layer thus formed was dried over magnesium sulfate, concentrated in vacuo, and purified by column chromatography (Hexane:EtOAc=3:1?2:1) to afford the title compound (64.9 mg, 79.7%) 1H NMR (400 MHz, CDCl3) delta 7.47-7.38 (m, 5H), 7.28-7.24 (m, 3H), 6.01 (s, 1H), 6.00 (brs, 1H), 4.32 (d, J=6.04 Hz, 2H), 2.39 (d, J=7.14 Hz, 2H), 1.75-1.69 (m, 1H), 0.81 (d, J=6.64 Hz, 6H) 13C NMR (100 MHz, CDCl3) delta 147.3, 144.2, 139.6, 135.7, 135.0, 132.2, 131.2, 129.1, 128.1, 125.5, 104.9, 41.3, 35.0, 28.3, 22.4

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; KOREA INSTITUTE OF SCIENCE AND TECHNOLOGY; NAM, Ghil Soo; CHOI, Kyung Il; KIM, Jung Hyun; PAE, Ae Nim; HONG, Jin Ri; LEE, Jae Kyun; (30 pag.)US2015/329533; (2015); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 53531-69-4, These common heterocyclic compound, 53531-69-4, name is (4-Bromophenyl)methanesulfonyl 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.

A solution of triphenylphosphine (5.13 g) and methylamine (2 M in tetrahydrofuran; 9.78 mL) in dichloromethane (10 mL) is added via a dosing pump over a period of 1 h to a mixture of 4-bromobenzylsulfonyl chloride (5.00 g) und triethylamine (5.45 mL) in dichloromethane (75 mL) at 0C under an argon atmosphere and the resulting mixture is stirred for 1 h at 0C. The reaction mixture is concentrated in vacuo and the residue is chromatographed on silica gel (cyclohexane/ethyl acetate 60:40?0:100) to give the title compound. LC (method 1 ): tR = 0.84 min; Mass spectrum (ESI+): m/z = 234, 236 [M+H]+.

Statistics shows that (4-Bromophenyl)methanesulfonyl chloride is playing an increasingly important role. we look forward to future research findings about 53531-69-4.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; LANGKOPF, Elke; BLUM, Andreas; (89 pag.)WO2016/23789; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 873-38-1, A common heterocyclic compound, 873-38-1, name is 2-Bromo-4-chloroaniline, molecular formula is C6H5BrClN, 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: A mixture of 2-iodoanilines (1.0 mmol), THF (3 mL), and t-BuOK (3 mmol) was stirred in a 10-mL sealed Schlenk tube for 5 min, and then dimethylthiocarbamoyl chloride (1.2 mmol) and CuBr (10 mol %) were added. The reaction mixture was heated at 60 C until completion as indicated by TLC. Then the mixture was cooled down to room temperature and quenched with sat. NH4Cl solution (5 mL). The aqueous phase was extracted with EtOAc (3 x10 mL). The combined organic phases were dried (Na2SO4), and the solvent was removed under reduced pressure. The obtained crude product was purified by flash column chromatography.

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; Chang, Cai-Zhu; Xu, Wan; Zeng, Meng-Tian; Liu, Min; Liu, Xing; Zhu, Hui; Dong, Zhi-Bing; Synthetic Communications; vol. 47; 13; (2017); p. 1262 – 1267;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics