Category: bromides-buliding-blocks

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. 7766-50-9, name is 11-Bromo-1-undecene, A new synthetic method of this compound is introduced below., Computed Properties of C11H21Br

[0129] 86 mmol of 1 1 -bromo1 -undecene and 91 mmol of triethoxy silane were added to a single neck RBF attached with an attached reflux condenser. Then 1.0 mL Karstedt’s catalyst (2 Wt. % solution in toluene, 0.1 mmol)) was added via syringe and flask was in the oil bath between 70 C for 2h. 1H NMR of the crude mixture showed a complete consumption of chain end olefin groups, however, a close examination of the spectrum showed presence of -15-20% olefin rearrangement products. Separation of (1 1 – bromoundecyl) triethoxysilane from rearrangement olefin and excess triethoxy silane was achieved by fractional distillation under high vacuum (Yield 67%).

The synthetic route of 7766-50-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK PATENT GMBH; BOBADE, Sachin; POLISHCHUK, Orest; PADMANABAN, Munirathna; BASKARAN, Durairaj; (65 pag.)WO2019/81450; (2019); 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. 75024-22-5, name is 1,4-Dibromo-2,3-dimethylbenzene, A new synthetic method of this compound is introduced below., Computed Properties of C8H8Br2

General procedure (a): A solution of 1,2-dimethylaryle 2b-e,h (10 mmol) and finely pulverised N-bromosuccinimide (NBS 3.68 g, 21 mmol, 2.1 equiv) in CCl4 (40-80 mL) was irradiated with HPK125 mercury lamp for 1-2 h with good stirring (tlc or 1H NMR monitoring). The reaction mixture was diluted with CH2Cl2, washed with H2O or 2 N aqueous NH4Cl solution and dried over MgSO4. The solvent was evaporated to give quantitatively 5b-e,h which was used without further purification.

The synthetic route of 75024-22-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Maiereanu, Carmen; Schmitt, Celine; Schifano-Faux, Nadge; Le Nouen, Didier; Defoin, Albert; Tarnus, Celine; Bioorganic and Medicinal Chemistry; vol. 19; 18; (2011); p. 5716 – 5733;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 21120-91-2, name is 7-Bromobicyclo[4.2.0]octa-1,3,5-triene, 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. HPLC of Formula: C8H7Br

To a stirred solution of mercury(II) oxide (591.3 mg, 2.73 mmol) and 35 % aqueous tetrafluoroboric acid (TFBA) (999.4 mg, 5.46 mmol) in 1,4-dioxane (10.9 mL), 1- bromobenzocyclobutene (1.0 g, 5.46 mmol) was added. The reaction stirred at room temperature for 2 h and was then treated successively with NaHCO3 and 3N KOH until the solution remained basic. The precipitated mercury(II) oxide was filtered off and the filtrate extracted with CH2Cl2 (3 x 300 mL), dried with anhydrous Na2SO4, filtered, and concentrated to yield white crystals that were purified via column chromatography using a 3:2 Hexanes:EtOAc solvent system.

The synthetic route of 7-Bromobicyclo[4.2.0]octa-1,3,5-triene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; VANDERBILT UNIVERSITY; WO2008/24435; (2008); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 7073-94-1, name is 1-Bromo-2-isopropylbenzene, belongs to bromides-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 7073-94-1, Product Details of 7073-94-1

To a solution of 1-bromo-2-isopropylbenzene (300 mg, 1.51 mmol) in dry THF (4.0 mL) cooled at -78 C, n-BuLi (1.6 M in n-hexane, 1.04 mL, 1.66 mmol) was added dropwise over 20 min. The mixturewas stirred for 15 min and dry DMF (128muL, 1.66 mmol) was slowly added at -78 C. After 15 minthe temperature was raised up to -10 C and water was added. The mixture was extracted 3 timeswith dichloromethane (5 mL), and the combined organic layers were dried over anhydrous Na2SO4,filtered and concentrated. The residue was purified by flash chromatography on silica gel (1:20 ethylacetate/petroleum ether), to give 10SI as a colorless oil (61% yield). 1H NMR (300 MHz, CDCl3): delta10.36 (s, 1H), 7.81 (d, 1H, J = 7.8 Hz), 7.55 (t, 1H, J = 7.5 Hz), 7.44 (d, 1H, J = 4.8 Hz), 7.34 (t, 1H, J =7.5 Hz), 4.01 – 3.95 (m, 1H), 1.32 (s, 3H), 1.25 (s, 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, 1-Bromo-2-isopropylbenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; D’Alessandro, Sarah; Alfano, Gloria; Di Cerbo, Luisa; Brogi, Simone; Chemi, Giulia; Relitti, Nicola; Brindisi, Margherita; Lamponi, Stefania; Novellino, Ettore; Campiani, Giuseppe; Gemma, Sandra; Basilico, Nicoletta; Taramelli, Donatella; Baratto, Maria Camilla; Pogni, Rebecca; Butini, Stefania; Bioorganic Chemistry; vol. 89; (2019);,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 14922-91-9, A common heterocyclic compound, 14922-91-9, name is 5-Bromo-2-ethylaniline, molecular formula is C8H10BrN, 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.

Step 2: Preparation of 4-bromo-1-ethyl-2-iodobenzeneTo a stirred mixture of 5-bromo-2-ethylaniline (3.39 g, 200 mmol) in distilled water (110 ml) is added concentrated sulfuric acid (5.60 ml), followed by brief heating at reflux until dissolution. The mixture is allowed to cool to room temperature, producing a fine precipitate, then further cooled to approximately 0 C. in an ice/salt bath. To this slurry is added an aqueous solution of sodium nitrite (1.17 g, 16.94 mmol) in distilled water (10 ml) dropwise over 15 minutes, maintaining a temperature below 5 C., followed by additional stirring for 30 minutes. The reaction mixture is next filtered then added to a second solution of aqueous potassium iodide (8.44 g, 50.83 mmol) in distilled water (45 ml) dropwise at room temperature. After the addition is complete the solution is briefly heated to 80 C. then allowed to cool to room temperature again. The reaction mixture is extracted with ethyl acetate (3×50 ml), and the organic phase is washed with 1M aqueous hydrochloric acid (30 ml) and aqueous sodium thiosulfate (2×30 ml). After drying over anhydrous magnesium sulfate and concentration in vacuo 4-bromo-1-ethyl-2-iodobenzene (4.90 g) is furnished as an orange liquid.

The synthetic route of 14922-91-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SYNGENTA CROP PROTECTION LLC; US2012/190545; (2012); 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. 5433-01-2, name is 1-Bromo-3-isopropylbenzene, A new synthetic method of this compound is introduced below., Safety of 1-Bromo-3-isopropylbenzene

A solution of 3-bromoisopropylbenzene (25 mmol) in 20 ml_ of dry THF was added dropwise over 20 min to 1.22 g (50 mmol) of magnesium turnings in 10 mL of refluxing THF under nitrogen and the mixture was refluxed for an additional 25 min to form the Grignard reagent. The Grignard solution was cooled and added by cannula to a suspension of CuBr-dimethylsulfide complex (0.52 g, 2.5 mmol) in dry THF at -25 C. The suspension was stirred at -25 C for 20 min, and then a solution of 1,4 cyclohexanedione, monoethylene ketal (3.9 g, 25 mmol) in 15 mL of THF was added dropwise over 5 min. The mixture was allowed to gradually warm to ambient temperature. After chromatography over silica gel, eluting with 20% to 30% ethyl acetate in heptane, alcohol 9 (5.6 g, 20 mmol, 80%) was isolated as a colorless oil which crystallized to a white solid on cooling: 1H NMR (CDCI3) 8 7.39 (s, 1 H), 7.33 (m, 1 H), 7.28 (t, J= 7.5 Hz, 1 H), 7.13 (d, J= 7.5 Hz, 1 H), 4.0 (m, 4 H), 2.91 (hept, J=7Hz, 1 H), 2.15(171, 4 H), 1.82 (br d, J= 11.5 Hz, 2 H), 1.70 (br d, J= 11.5 Hz, 2 H), 1.25 (d, J = 7 Hz, 6 H); MS (Cl) m/z 259.2 (M-OH).

The synthetic route of 5433-01-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ELAN PHARMACEUTICALS INC.; WO2006/10095; (2006); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 1422-54-4, name is 2-Bromo-6-fluorotoluene, belongs to bromides-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 1422-54-4, SDS of cas: 1422-54-4

To a solution of 1-bromo-3-fluoro-2-methylbenzene (2.0 g, 10.6 mmol) in N,N- dimethylformamide (10 ml) was added sodium methanethiolate (0.85 g, 11.7 mmol) and the mixture was stirred for 15 min at 150 C. After cooling, aqueous sodium carbonate (10%, 50 ml) was added and the phases were separated. The aqueous phase was extracted with ethylacetate (2×50 ml) and the combined organic phases was dried (MgS04) and evaporated under reduced pressure to give an oil. The residue was purified by flash column chromatography (isooctane) to give the title compound (1.33 g). MS m/z (relative intensity, 70 eV) 218 (M+, 98), 216 (M+, 92), 202 (26), 200 (26), 122 (bp), 121 (56).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Bromo-6-fluorotoluene, and friends who are interested can also refer to it.

Reference:
Patent; A. CARLSSON RESEARCH AB; WO2005/121087; (2005); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 61326-44-1, 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. 61326-44-1 name is 1,1,2,2-Tetrakis(4-bromophenyl)ethene, 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.

In a polar solvent, 1,1,2,2-tetrakis (4-bromophenyl) ethylene, 1,1,2,2-tetrakis (4-bromophenyl)1H-1,2,4-triazole,Potassium carbonate andCopper oxide in the reaction conditions;Wherein 1,1,2,2-tetrakis (4-bromophenyl) ethylene:1H-1,2,4-triazole:Potassium carbonate:The molar ratio of copper oxide is 2: 10-15: 30: 1;The reaction temperature is 80-200 DEG C, the reaction time is 12-120 hoursThe present invention is preferably 1,1,2,2-tetrakis (4-bromophenyl) ethylene:1H-1,2,4-triazole:Potassium carbonate:The molar ratio of copper oxide was2: 10-15: 30: 1;Reaction temperature 100 ,The reaction time was 48 hours.In a polar solvent,Using the “one-pot method”1, 1, 2,(4-bromophenyl) ethene, 1H-1,2,4-triazole, potassium carbonate and copper oxide were heated under heating to produce 1,1,2,2-tetrakis [4-(1H-1,2,4-triazol-1-yl) phenyl] ethylene (L). Yield 60percent.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,1,2,2-Tetrakis(4-bromophenyl)ethene, and friends who are interested can also refer to it.

Reference:
Patent; Tianjin Normal University; Wang, Ying; (11 pag.)CN105524086; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 24358-62-1, A common heterocyclic compound, 24358-62-1, name is 1-(4-Bromophenyl)ethylamine, molecular formula is C8H10BrN, 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.

First, N-(1-(4-(2,5-bicyclo[2.2.1]heptenyl) phenyl)ethyl)maleimide was synthesized in three stages. 1-(4-Bromophenyl)ethylamine (25.1 g, 0.125 mol) was dissolved in diethyl ether (100 mL), and slowly added dropwise at 0 C. to a diethyl ether solution (200 mL) of maleic anhydride (10.4 g, 0.106 mol). The reaction solution was stirred for two hours at room temperature, and the solid that precipitated was filtered out and washed several times by diethyl ether. The solid filtered out and sodium acetate (1.20 g) were dissolved in acetic anhydride (120 mL), and stirred for four hours at 140 C. The solvent was distilled off under reduced pressure, water was added, and the solution was extracted by methylene chloride. The organic layer was dried using anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography using chloroform-hexane mixed solvent (mixture ratio 4:1) as the developing solvent, and N-(1-(4-bromophenyl)ethyl)maleimide (23.5 g, 84.0 mmol, 79%) was obtained as a white solid. The spectra data of N-(1-(4-bromophenyl)ethyl)maleimide were as follows. 1H NMR (400 MHz, CDCl3): delta 7.46-7.43 (m, 2H), 7.31-7.28 (m, 2H), 6.64 (s, 2H), 5.30 (q, J=7.6 Hz, 1H), 1.79 (d, J=7.6 Hz, 3H); 13C NMR (100 MHz, CDCl3): delta 170.3, 139.1, 140.0, 131.5, 129.0, 121.6, 48.9, 17.4; HRMS (APCI, positive): [M+] calcd. for C12H10BrNO2, 278.9895; found 278.9904.

The synthetic route of 24358-62-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Japan Science and Technology Agency; Yabu, Hiroshi; Saito, Yuta; Saito, Shohei; Yamaguchi, Shigehiro; Nobusue, Shunpei; (47 pag.)US10442886; (2019); B2;,
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. 1003-99-2, name is 2-Bromo-5-fluoroaniline, A new synthetic method of this compound is introduced below., Formula: C6H5BrFN

EXAMPLE 4 2-(2-amino-4-fluorophenyl)-3-methyl-2-cyclopenten-1-one 4.937 g (25.982 mmol) of 2-bromo-4-fluoroaniline, 4.00 g (28.584 mmol) of 5-methyl-1-cyclopenten-2-one boronic acid compound, 0.30 g (0.260 mmol) of tetrakis(triphenylphosphine)palladium, and 4.13 g (38.978 mmol) of sodium carbonate were loaded to 250 mL schlenk flask, and then 80 mL of degassing DME and 27 mL of H2O that had been purged with N2 were added thereto using a syringe. The mixture was reacted at 90° C. for 12 hours. The work-up was the same as in Example 3 (3.84 g, 72percent). 1H NMR (CDCl3): =6.83 (t, J=7.6 Hz, 1H, Ph), 6.48 (t, J=7.6 Hz, 1H, Ph), 6.43 (d, J=10.4 Hz, 1H, Ph), 3.82 (br s, 2H, NH2), 2.73-2.71 (m, 2H, CH2CP), 2.58-2.55 (m, 2H, CH2Cp), 2.09 (s, 3H, CH3); 13C {1H} NMR (CDCl3): =207.93, 175.26, 168.18(d, J=242.6 Hz, PhC-F) 146.47(d, J=5.7 Hz, Ph), 138.76, 131.90(d, J=9.8 Hz, Ph), 113.71, 105.08(d, 22 Hz, Ph), 102.91 (d, 22 Hz, Ph), 34.79, 32.22, 18.63

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; LG Chem, Ltd.; US7538239; (2009); B2;,
Bromide – Wikipedia,
bromide – Wiktionary