Category: 4263-52-9

Synthetic Route of 4263-52-9, A common heterocyclic compound, 4263-52-9, name is Sodium 2-bromoethanesulphonate, molecular formula is C2H4BrNaO3S, 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 solution of 1mmol of chloride salt 1a or 2a in distilled water was treated with equimolar quantity of various salts (NaBF4, KPF6, 2-BrCH2CH2SO3Na). The reaction mixture was stirred at room temperature for 12h. Next, the reaction mixture was extracted twice with CH2Cl2. The organic layer was dried over anhydrous Na2SO4 and then CH2Cl2 was evaporated on a rotary evaporator to give various chiral ionic liquids 1b-d and 2b-d. 4.4.6 1-[(-)-Borneoxycarbonylmethylene]-3-methyl benzimidazolium 2-bromoethylsulfonate [ABoMBI]OSO2CH2CH2Br 2d Off-white solid Yield = 83%, mp = 96-98 C, [alpha]D25 = -15.6 (c 0.25, EtOH). 1H NMR (CDCl3, 400 MHz): delta 10. 35 (s, 1H), 7.78-7.68 (d, 1H, Ar), 7.60 (s, 3H, Ar), 5.47 (s, 2H NCH2), 5.44-5.35 (d, 1 H), 4.13 (s, 3H N-CH3), 3.60-3.52 (t, 2H), 3.20-3.07 (t, 2H), 2.31-2.19 (m, 1H), 1.72-1.56 (m, 3H), 1.19 (s, 3H), 1.02-0.97 (d, 1H), 0.80 (s, 6H), 0.74 (s, 3H). 13C NMR (CDCl3, 400 MHz): delta 166.09, 144.39, 131.67, 131.47, 127.46, 127.32, 113.07, 112.93, 83.16, 54.40, 48.93, 47.91, 44.64, 36.34, 33.76, 29.59, 27.79, 26.87, 26.29, 19.58, 18.72, 13.47. EI-MS: m/z = 327 [M+cation], m/z = 312 [M+cation-CH3].

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; Singh, Avtar; Chopra, Harish Kumar; Tetrahedron Asymmetry; vol. 27; 11-12; (2016); p. 448 – 453;,
Bromide – Wikipedia,
bromide – Wiktionary

4263-52-9, A common compound: 4263-52-9, name is Sodium 2-bromoethanesulphonate, belongs to bromides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below.

Potassium O-ethylxanthate (3 x 95mg, O.deltaOmmol) is added portion wise every 1 .5 hours to a solution of sodium 2-bromoethanesulphonate (0.42g, 2.00mmol) in acetonitrile (15ml). The reaction mixture is heated at 850C, under a nitrogen atmosphere, for a total of 6 hours. Upon cooling the suspension is filtered, washed with acetonitrile and air-dried affording an off-white solid.1 H NMR (DMSO d6) delta (ppm) 4.67 (q, 2H), 3.40 (2H, m), 3.26 (m, 2H), 1 .39 (t, 3H).

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, Sodium 2-bromoethanesulphonate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; UCB PHARMA S.A.; WO2009/19119; (2009); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 4263-52-9, 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. 4263-52-9, name is Sodium 2-bromoethanesulphonate, This compound has unique chemical properties. The synthetic route is as follows.

Synthesis of intermediate II (1-delta-sulphoethyl,-2,3,3-trimethyl-5-sulphonamido indolenininium inner salt); [Show Image] 150 g of 2-bromoethanesulfonic acid sodium salt, Fluka, 1,5 1 of ethanol are mixed together, the mixture is then cooled to 5C and 29,2 g of hydrochloric acid gas are bubbled through the mixture. After that, the mixture is brought back to RT and left under stirring for 4 hours. After filtration of sodium chloride, the mixture is concentrated to dryness under vacuum. 1,6 g of 2-bromoethanesulfonic acid, obtained with the method reported above, 1,3 g of intermediate I, 0,7 g of triethylamine and 5 ml of butirronitrile are mixed together and heated to reflux for 20 hours. The mixture is then cooled to rrom temperature and 15 ml of acetone are added. The solid product is vacuum filtered and washed with methanol and acetone. The reaction yield is 50%.

The chemical industry reduces the impact on the environment during synthesis Sodium 2-bromoethanesulphonate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Ferrania Technologies S.p.A.; EP1810998; (2007); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 4263-52-9, name is Sodium 2-bromoethanesulphonate, A new synthetic method of this compound is introduced below., Product Details of 4263-52-9

A solution OF 2-BROMOETHANESULFONIC acid, sodium salt (4.2 g, 20 mmol) in water (total 12 ML) was added over 6 hours to a 42 C solution oft-butylamine (10 mL, 94 mmol) in a mixture of water (10 mL) and 1,4-dioxane (10 mL). The mixture was stirred at 42 FOR 18 hours. The mixture was then heated to 60 C for 24h. By proton NMR, 30 % of elimination product (vinylsulfonic acid) was observed. The mixture was concentrated to dryness and treated with ethanol at refluxing temperature. The solid material was collected (crop 1). The mother liquor was concentrated to dryness and the solid was again treated with ethanol at refluxing temperature, and the solid material was collected (crop 2). Both crops of the solid material were dissolved in water, and the resultant aqueous solutions passed in sequence through a Dowex 50 W X 8 ion- exchange column (100 g resin). The fractions containing the title compound were collected and concentrated to dryness. The solid material obtained was recrystallized from a mixture of ethanol (20 mL) and water (2 mL). The crystals were collected by filtration, dried in a vacuum oven at 60 C for 18 hours. Compound DU was obtained as fine white needles (860 mg, 24 % YIELD). 1H NMR (500 MHz, D20) B 1.16 (s, 9H), 3.02 (t, J= 6. 8 Hz, 2H), 3.19 (t, J= 6. 8 Hz, 2H). 13C NMR (125 MHz, D20) 8 24. 8, 37. 3,47. 0,57. 8. ES-MS 182 (M+1)

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; NEUROCHEM (INTERNATIONAL) LIMITED; WO2004/113275; (2004); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 4263-52-9, name is Sodium 2-bromoethanesulphonate, This compound has unique chemical properties. The synthetic route is as follows., name: Sodium 2-bromoethanesulphonate

Phosphorus pentachloride (commercially available, for example, from Aldrich) (1 1.8 g, 57 mmol) was added portionwise to stirred sodium bromoethanesulfonate (commercially available, for example, from Aldrich) (4.0 g, 19 mmol) over five minutes. When the addition was complete, the suspension was heated to 1 10 0C for 2 h before cooling to 21 0C and then pouring onto ice. The product was extracted with dichloromethane and the organic layer was washed successively with water, sodium bicarbonate and water. The organic solution was dried over magnesium sulfate and evaporated to give the title compound (3.24 g), 1H NMR delta (CDCI3) 4.12 (2H, t, J = 8 Hz), 3.79 (2H, t, J = 8 Hz).

According to the analysis of related databases, 4263-52-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GLAXO GROUP LIMITED; WO2009/47336; (2009); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 4263-52-9, name is Sodium 2-bromoethanesulphonate, A new synthetic method of this compound is introduced below., HPLC of Formula: C2H4BrNaO3S

44.6 g of isophorone diisocyanate (IPDI) was added in a mechanically agitated round-bottom flask. 0.2 mL of catalyst dibutyltin dilaurate was added in the IPDI, and 17.8 g of dimethyl ethanolamine (HO CH2CH2N(CH3)2) was added dropwise in the IPDI while stirring at 30 C. using a dropping funnel to form a reaction mixture. The reaction mixture reacted for 1 hr, and then was stirred to react for 12 hrs at 30 C. 42.2 g of 2-bromoethyl sodium sulfonate which was dissolved in 400 mL of anhydrous tetrahydrofuran was added dropwise in the reaction mixture and reacted for 1 hr to yield a white precipitate. The white precipitate was centrifugalized several times to yield the isocyanate-terminated betaine compound.

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; Shenzhen University; CHEN, Shiguo; YUAN, Lingjun; ZHU, Xingli; CHEN, Shaojun; GE, Zaochuan; (11 pag.)US2017/339960; (2017); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 4263-52-9, A common heterocyclic compound, 4263-52-9, name is Sodium 2-bromoethanesulphonate, molecular formula is C2H4BrNaO3S, 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 solution of 1mmol of chloride salt 1a or 2a in distilled water was treated with equimolar quantity of various salts (NaBF4, KPF6, 2-BrCH2CH2SO3Na). The reaction mixture was stirred at room temperature for 12h. Next, the reaction mixture was extracted twice with CH2Cl2. The organic layer was dried over anhydrous Na2SO4 and then CH2Cl2 was evaporated on a rotary evaporator to give various chiral ionic liquids 1b-d and 2b-d. 4.4.6 1-[(-)-Borneoxycarbonylmethylene]-3-methyl benzimidazolium 2-bromoethylsulfonate [ABoMBI]OSO2CH2CH2Br 2d Off-white solid Yield = 83%, mp = 96-98 C, [alpha]D25 = -15.6 (c 0.25, EtOH). 1H NMR (CDCl3, 400 MHz): delta 10. 35 (s, 1H), 7.78-7.68 (d, 1H, Ar), 7.60 (s, 3H, Ar), 5.47 (s, 2H NCH2), 5.44-5.35 (d, 1 H), 4.13 (s, 3H N-CH3), 3.60-3.52 (t, 2H), 3.20-3.07 (t, 2H), 2.31-2.19 (m, 1H), 1.72-1.56 (m, 3H), 1.19 (s, 3H), 1.02-0.97 (d, 1H), 0.80 (s, 6H), 0.74 (s, 3H). 13C NMR (CDCl3, 400 MHz): delta 166.09, 144.39, 131.67, 131.47, 127.46, 127.32, 113.07, 112.93, 83.16, 54.40, 48.93, 47.91, 44.64, 36.34, 33.76, 29.59, 27.79, 26.87, 26.29, 19.58, 18.72, 13.47. EI-MS: m/z = 327 [M+cation], m/z = 312 [M+cation-CH3].

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; Singh, Avtar; Chopra, Harish Kumar; Tetrahedron Asymmetry; vol. 27; 11-12; (2016); p. 448 – 453;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 4263-52-9, 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. 4263-52-9, name is Sodium 2-bromoethanesulphonate belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A mixture of 1-(2,2-diferrocenylpropane) methyl-imidazole (1.68g, 3.42mmol) and sodium 2-bromoethanesulphonate (0.72g, 3.42mmol) were refluxed at 80C for 16h in DMF (50mL). After cooling to room temperature, the reaction mixture was washed with H2O, and partitioned between H2O and CH2Cl2. The combined organic extract was dried (MgSO4) and concentrated. The residue was purified by silica gel (100-200mesh) chromatography to yield 2 (0.68g, 28%) as an orange-yellow solid. M.p. 46-47C. 1H NMR (400MHz, CDCl3): delta 9.22 (d, 1H, J=28.4Hz, NCHN), 7.50 (d, 1H, J=14.4Hz, NCH), 7.07 (d, 1H, J=7.6Hz, NCH), 5.10 (d, 2H, J=60.4Hz, CH2), 4.59 (s, 2H, CH2), 4.35-3.97 (m, 17H, Cp-H), 3.33 (s, 2H, CH2), 1.66-1.42 (m, 6H, CH3). 13C NMR (101MHz, CDCl3): delta 136.53 (N=C), 122.84 (N=C), 120.82 (N=C), 103.35 (N-CH2-Cp), 102.71 (N-CH2), 78.65 (Cp), 78.38 (Cp), 69.75 (Cp), 69.02 (Cp), 68.18 (Cp), 66,94 (Cp), 50.68 (Cp), 49.78 (Cp), 46.62 (CH2), 33.11 (CH3), 30.50 (CH3). MS (ESI) m/z 701.75 [M]+, 622.83 [M-Br]+, 599.08 [M-Br-Na]+, 78.83 [Br]- Cal. 702. IR (KBr cm-1): upsilon 3094 (=C-H), 2973 (C-H), 1640 (C=C), 1562 (C=N), 1447 (S=O), 1357, 1201, 1106, 1042, 1001, 817, 739, 479. HRMS (M-Br-Na)+: calcd 600.0828, obsd 600.0822.

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, Sodium 2-bromoethanesulphonate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Su, Zhi-Ming; Ye, Hong-Min; Zhu, Xiao-Xiao; Xie, Li-Li; Bai, Sha; Yuan, Yao-Feng; Journal of Organometallic Chemistry; vol. 750; (2014); p. 162 – 168;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 4263-52-9, name is Sodium 2-bromoethanesulphonate, 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. Quality Control of Sodium 2-bromoethanesulphonate

b) Compound lb; [0169] A mixture of compound la, (0.1 g, 0.45 mmole), sodium 2- bromoethanesulfonate (0.19 g, 2 equivalents) and 2,6-di-tert-butylpyridine (99 muL, 0.45 mmole) in [BMIM]BF4] (1 mL, Aldrich) was heated in an oil bath at 150C with vigorous stirring for 16 hours. The reaction was then cooled to room temperature and a small portion of the reaction mixture was withdrawn, diluted with methanol/water and analyzed by analytical HPLC using a Phenomenex, Ci8,4.6 x 250 mm column and a 30 minute gradient of 10? 70% MeCN/water (with 0.05% TFA) at a flow rate of 1.0 mL/minute and UV detection at 260nm and 220 nm. Product was observed eluting at Rt = 13.3 minutes (-40% conversion). The reaction mixture was prepared by diluting it with water (15 mL) and washing this solution with ethyl acetate (2 x 25 mL). The aqueous solution was then treated with 3 to 4 drops of ammonia and further extracted with ethyl acetate (2 x 25 mL). The aqueous solution was then concentrated to about 7 mL by rotary evaporation. The product was then purified by preparative HPLC using an YMC, Ci8, 30 x 250 mm column and the same gradient as described above at a flow rate of 20 mL/minute. HPLC fractions containing product were combined and concentrated under reduced pressure. Yield = 30 mg (20%, white solid); MALDI-TOF MS 330.6 observed.

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

Reference:
Patent; SIEMENS HEALTHCARE DIAGNOSTICS INC.; NATRAJAN, Anand; SHARPE, David; WEN, David; JIANG, Qingping; WO2011/146595; (2011); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 4263-52-9, 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. 4263-52-9, name is Sodium 2-bromoethanesulphonate, This compound has unique chemical properties. The synthetic route is as follows.

Synthesis of intermediate II (1-delta-sulphoethyl,-2,3,3-trimethyl-5-sulphonamido indolenininium inner salt); [Show Image] 150 g of 2-bromoethanesulfonic acid sodium salt, Fluka, 1,5 1 of ethanol are mixed together, the mixture is then cooled to 5C and 29,2 g of hydrochloric acid gas are bubbled through the mixture. After that, the mixture is brought back to RT and left under stirring for 4 hours. After filtration of sodium chloride, the mixture is concentrated to dryness under vacuum. 1,6 g of 2-bromoethanesulfonic acid, obtained with the method reported above, 1,3 g of intermediate I, 0,7 g of triethylamine and 5 ml of butirronitrile are mixed together and heated to reflux for 20 hours. The mixture is then cooled to rrom temperature and 15 ml of acetone are added. The solid product is vacuum filtered and washed with methanol and acetone. The reaction yield is 50%.

The chemical industry reduces the impact on the environment during synthesis Sodium 2-bromoethanesulphonate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Ferrania Technologies S.p.A.; EP1810998; (2007); A2;,
Bromide – Wikipedia,
bromide – Wiktionary