Month: August 2021

Synthetic Route of 2695-47-8, 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. 2695-47-8, name is 6-Bromo-1-hexene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Synthesis of 2-(4-bromobutyl)-oxirane (I): A Solution of 3- Chloroperbenzoic acid (55-75% pure, 4.54 g, 18.39 mmol) in 20 ml dichloromethane was added dropwise to a stirred solution of 6-bromo-l-hexne (2g, 12.26 mmol) in 20 ml of dichioromethane. After addition, the mixture was stirred at 25 C for 16h, to precipitate 3-chiorobenzoic acid. Finally the reaction mixture was evaporated to dryness under vacuum, dissolved in ethyl acetate, washed initially with 4% sodium dithionate followed by saturated sodium bicarbonate and water. Finally the organic layer was dried over sodium sulphate, evaporated and dried under vacuo to obtain the final compound (I) with 90% isolated yield. -NMR (400 MHz, CDC13) delta ppm: -NMR (400 MHz, CDC13) delta ppm: 1 .48- 1 .6(6H, m, CH2) 2.47 ( 1 H, d, J = 2.4, OCH) 2.75 (t, J = 4, 1 H, OCHb), 2.91 (bs, 1 H, OCHa) 3.41 (t, J = 6.4, 2H, CH2-Br) .

The synthetic route of 6-Bromo-1-hexene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; VYOME BIOSCIENCES PVT. LTD.; SENGUPTA, Shiladitya; CHAWRAI, Suresh Rameshlal; GHOSH, Shamik; GHOSH, Sumana; JAIN, Nilu; SADHASIVAM, Suresh; BUCHTA, Richard; BHATTACHARYYA, Anamika; WO2015/114666; (2015); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 67567-26-4, 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. 67567-26-4, name is 4-Bromo-2,6-difluoroaniline belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A solution of 4-bromo-2,6-difluoroaniline (240 mmol) inAcOR (150 mE) was added dropwise to a suspension ofNa1303.4 H20 (325 mmol) in AcOR (450 mE) at 70 C. during 30 mi Another 2080 mmol of Na1303.4 H20 were added over 5 h to the mixture. During this period the mixturewas stirred at 70 C. The mixture was poured into water andextracted with Et20. The organic layer was combined withanother Et20 solution obtained from another reaction using the same conditions described above. The mixture was concentrated. A precipitate was formed and separated by filtration. The filtrate was concentrated to afford the desired product after flash column chromatography (Si02, petroleum ether).

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-Bromo-2,6-difluoroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GALAPAGOS NV; Menet, Christel Jeanne Marie; Mammoliti, Oscar; Blanc, Javier; Orsulic, Mislav; Roscic, Maja; (81 pag.)US9440929; (2016); B2;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 327-51-5, name is 1,4-Dibromo-2,5-difluorobenzene, 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 327-51-5, Quality Control of 1,4-Dibromo-2,5-difluorobenzene

Freshly titrated n-butyl lithium (27. 0 ml, 1. 39 M in hexanes) is added slowly (over about 30 minutes) to a-78 C solution of diethyl ether (90 ml) containing 1, 4-dibromo- 2, 5-DIFLUOROBENZENE (1, 10. 22 g, 0. 038 mol). The resulting yellow solution is stirred at-78 C for 2 hours to give a yellow suspension. Several pellets (-10) of dry ice are added to the suspension, which is then allowed to warm slowly to room temperature as it degasses (approximately 40 minutes). The resulting suspension is acidified with a 1 M aqueous solution of hydrochloric acid (500 ml), and the product extracted with diethyl ether (5 x 200 ml). The combined organics are washed with water (4 x 100 ml) and filtered. The ether solution is concentrated to approximately 200 ml under reduced pressure, and the product extracted into a saturated aqueous solution of sodium bicarbonate (3 x 200 ml). The combined aqueous extracts are washed with methylene chloride (3 x 100 ml) and acidified with hydrochloric acid. The product is extracted with diethyl ether (3 x 200 ml), and the combined organic extracts washed with water (2 x 200 ml), dried over magnesium sulfate, and concentrated under reduced pressure to give (2) as a pale yellow SOLID. 1H NMR (300 MHz, DMSO-d6) : 5 7. 74 (dd, JH-F = 8. 5 Hz, 6. 5 Hz, 1H), 7. 84 (DD, JH-F = 10. 0 Hz, 5. 5 Hz, 1H), 13. 7 (br, 1H, CO2H). 19F{1H} NMR (282 MHz, DMSO-d6) : No.-114. 0 (d, JF-F = 17. 0 Hz, 1F),-113. 6 (D, JF-F = 17. 0 Hz, 1F). I3C {LH} NMR (75 MHz, DMSO-D6) : No.113. 6 (dd, JC-F = 23. 5 Hz, 10. 0 Hz), 118. 4 (DD, JC-F = 26. 5 Hz, 2. 5 Hz, CH), 120. 0 (DD, JC-F = 19. 0 Hz, 12. 0 Hz), 122. 2 (D, JC-F = 28. 0 Hz, CH), 154. 4 (dd, JC-F = 245. 0 Hz, 5. 5 Hz, CF), 156. 8 (dd, JC-F = 251. 5 Hz, 4. 0 Hz, CF), 163. 4 (m, COXH).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,4-Dibromo-2,5-difluorobenzene, and friends who are interested can also refer to it.

Reference:
Patent; ACHILLION PHARMACEUTICALS, INC.; WO2005/19228; (2005); 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. 586-61-8, name is 1-Bromo-4-isopropylbenzene, A new synthetic method of this compound is introduced below., HPLC of Formula: C9H11Br

[00312j A mixture of 4-(benzyloxy)aniline (7.8 g, 39.03 mmol), 1-bromo-4- isopropylbenzene (8.5 g, 42.93 mmol), X-Phos (2.3 g, 4.68 mmol), Pd(OAc)2 (0.53 g, 2.34 mmol) and Cs2CO3 (50.9 g, 156.12 mmol) in toluene(150 mL) was purged with N2 and then reflux overnight. The reaction mixture was cooled to RT and filtered. The filtrate was concentrated and purified by silica column chromatography (PE:EA, 20:1) to give 7.1 g (57%) of the title compound. ?H NMR (CDC13, 300 MHz): oe 1.23 (d, J= 6.9 Hz, 6H), 2.77-2.92 (m, 1H), 5.04 (s, 2H), 6.87-6.94 (m, 4H), 7.01-7.04 (m, 2H), 7.08-7.10 (m, 2H), 7.3 1-7.46 (m, 5H). [M+H] Calc?d for C22H23N0, 318; Found, 318.

The synthetic route of 586-61-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; QUANTICEL PHARMACEUTICALS, INC.; BOLOOR, Amogh; KANOUNI, Toufike; STAFFORD, Jeffrey Alan; VEAL, James Marvin; WALLACE, Michael Brennan; (173 pag.)WO2016/44429; (2016); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 28342-75-8, name is 1,5-Dibromo-2,4-difluorobenzene, 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. Product Details of 28342-75-8

38. Preparation of 1-bromo-2,4-difluoro-5-methoxybenzene; To a solution of 1,3 dibromo-4,6-difluorobenzene (10.0 g, 37 mmol) in THF (50 mL) at -20° C. was added isopropyl magnesium chloride (2.0M in THF, 42 mmol) and the resulting solution warm to 0° C. and stirred for 30 minutes. Trimethylborate (4.7 g, 45 mmol) was added and the mixture stirred at ambient temperature for 1 hour. The solution was recooled to -20° C. and peracetic acid (32percent, 50 mmol) was added and the solution was stirred for 30 minutes at ambient temperature. The solution was then quenched with sodium bisulfite (5percent solution, 75 mL) and then acidified with 6 N hydrochloric acid and extracted with ethyl ether (2.x.75 mL). Combined extracts were dried (sodium sulfate) and concentrated. The crude phenol was dissolved in acetonitrile (40 mL) and potassium carbonate (10 g, 74 mmol) and iodomethane (5.7 g, 40 mmol) were added and stirred at ambient temperature for 20 hours. The solution was concentrated and the residue taken into water (50 mL) and extracted with ethyl ether (2.x.75 mL) and the combined extracts were washed with brine, dried (sodium sulfate), and concentrated. The residue was purified by chromatography (hexanes) to give 1-bromo-2,4-difluoro-5-methoxybenzene (2.0 g, 8.6 mmol): LC/MS (m/z=223).

The synthetic route of 1,5-Dibromo-2,4-difluorobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Balko, Terry W.; Schmitzer, Paul R.; Daeuble, John F.; Yerkes, Carla N.; Siddall, Thomas L.; US2007/179060; (2007); A1;,
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. 59734-92-8, name is 1-Bromo-2-cyclohexylbenzene, This compound has unique chemical properties. The synthetic route is as follows., category: bromides-buliding-blocks

A Schlenk tube was charged with Cul (9.6 mg, 0.050 mmol, 5.0 mol%), NaI (300 mg, 2.00 mmol), evacuated and backfilled with argon. Racemic [TRANS-N, N’-DIMETHYL-1,] 2- cyclohexanediamine (16 RL, 0.10 mmol, 10 mol%), 1-bromo-2-cyclohexylbenzene (97% pure; Lancaster; 186 [(IL,] 1.00 mmol), n-pentanol (1 mL) were added under argon. The Schlenk tube was sealed with a Teflon valve and the reaction mixture was stirred at [130 C] for 40 h. The resulting suspension was allowed to reach room temperature and filtered through silica gel (1 x0. 5 cm) eluting with hexane (50 mL). The filtrate was concentrated, and the residue was purified by flash chromatography on silica gel (hexane) to provide the known [1-IODO-2-CYCLOHEXYLBENZENE] (283 mg, 99% yield; ca. 97% pure) as a colorless liquid. [SEE MCGUINE,] T. H.; Dull, M. F. J. Am. [CHEM. SOC.] 1947, 69, [1469.’H NMR] (400 MHz, [CDC13)] : 8 7. 85 (dd, [J= 7.] 5,1. [2 HZ,] 1H), 7.32 (td, J= 7.5, 1. [2 HZ,] 1H), 7.23 (dd, [J= 7.] 5,1. [7 HZ,] 1H), 6.90 [(TD,] [J= 7.] 5,1. [7 HZ,] 1H), 2.81 (tt, J= 11.7, 3. [0 HZ, 1H),] 1.97-1. 74 (m, [5H),] 1.55-1. 23 (m, [5H).] [13CNMR] (100 MHz, [CDC13)] : 8 149.3, 139.5, 128.4, 127.6, 126.6, 101.5, 48. 5,33. 4,26. 8,26. 1.

According to the analysis of related databases, 59734-92-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; MASSACHUSETTS INSTITUTE OF TECHNOLOGY; WO2004/13094; (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. 627871-16-3, name is 5-Bromo-4-fluoro-2-methylaniline, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 627871-16-3

WXBB-1-4a (20.00 g, 98.02 mmol, 1.00 eq) was dissolved in N-methylpyrrolidone (100.00 mL), followed by addition of cuprous cyanide (17.56 g, 196.04 mmol, 42.83 mL, 2.00 eq). The reaction was carried out at 180C for 3 hours. The reaction solution was cooled to room temperature, followed by addition of water (300 mL) and ammonia (300 mL), stirred at room temperature for 30 minutes, and extracted with ethyl acetate (200 mL 3). The organic phase was washed with saturated brine (200 mL) and water (200 mL), dried over anhydrous sodium sulfate, suction-filtered and rotary evaporated to dry under reduced pressure to give a crude product as a brown-black solid. The crude product was isolated by silica gel column chromatography (PE: EA=20:1-3:1) to give WXBB-1-4 (12.00 g, 79.92 mmol, 81.53% yield) as a yellow solid. 1H NMR (400 MHz, CHLOROFORM-d) delta ppm 2.21 (s, 3 H) 3.68 (br s, 2 H) 6.80 (d, J=5.40 Hz, 1 H) 6.91 (d, J=9.29 Hz, 1 H).

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 627871-16-3.

Reference:
Patent; Fujian Cosunter Pharmaceutical Co., Ltd.; WU, Chengde; YU, Tao; LI, Ning; CHEN, Shuhui; (58 pag.)EP3572412; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 103-64-0, A common heterocyclic compound, 103-64-0, name is (2-Bromovinyl)benzene, molecular formula is C8H7Br, 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: Vinyl halide (0.3mmol, if it is solid), CuI (0.0001 mol%, 20 muL in DMSO), PPh3 (2mol%), K2CO3 (0.6mmol), and tetra n-butylammonium acetate were added to a screw-capped test tube with 3 mL of deoxygenated water. The tube was evacuated and backfilled with argon (3 cycles). Under the argon atmosphere, the alkyne (0.4 mmol) and vinyl halide (if it is liquid) were added by syringe at room temperature. The mixture was heated to 100C and stirred for 24 h. After cooling to room temperature, the mixture was extracted three times with ethyl acetate. The organic layers were combined, dried over Na2SO4, and concentrated to yield the crude product, which was further purified by silica gel chromatography, using petroleum ether and ethyl acetate as eluent to provide the desired product.

The synthetic route of 103-64-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Sun, Peng; Yan, Hong; Lu, Linhua; Liu, Defu; Rong, Guangwei; Mao, Jincheng; Tetrahedron; vol. 69; 34; (2013); p. 6969 – 6974;,
Bromide – Wikipedia,
bromide – Wiktionary

Some common heterocyclic compound, 141474-37-5, name is 2,4-Dibromo-6-fluoroaniline, molecular formula is C6H4Br2FN, 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. Product Details of 141474-37-5

5.38g (20.0 mmol) of 2,4-dibromo-6-fluoro-phenylamine, 5.36 g (44.0 mmol) of phenylboronic acid, 1.15 g (1.0 mmol) of Pd(PPh3)4, and 8.29 g (60.0 mmol) of K2CO3 were dissolved in 80 mL of a mixed solution THF/H2O (2:1) to obtain a solution, which was then stirred at about 70C for about 5 hours. The reaction solution was cooled to room temperature, followed by three times of extraction with 60 mL of water and 60 mL of diethylether. The organic phase was collected, and was dried using magnesium sulfate to evaporate the solvent. The residue was separated and purified using silica gel column chromatography to obtain 4.11 g of Intermediate I-29 (Yield: 78 %) This compound was identified using LC-MS and NMR. C18H14FN : M+ 263.1 1H NMR (CD2Cl2, 400MHz) delta (ppm) 7.62-7.57 (t, 1H), 7.56-7.54 (m, 1H), 7.51-7.47 (m, 4H), 7.44-7.37 (m, 3H), 7.31-7.30 (m, 1H), 7.29-7.26 (m, 1H), 7.23-7.22 (m, 1H), 3.94 (s, 2H)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 141474-37-5, its application will become more common.

Reference:
Patent; Samsung Mobile Display Co., Ltd.; EP2447250; (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. 460-00-4, name is 1-Bromo-4-fluorobenzene, A new synthetic method of this compound is introduced below., Safety of 1-Bromo-4-fluorobenzene

Synthesis of compound 42C10H7FS M = 178.23 g.mol”1 19F NMR (CDCh 282.5MHz): -109.8 (m, IF, Ar-F).Mass (GC-MS): 133 (41%); 178 (100%)Into a freshly degassed mixture of EtOH (69mL) and H20 (9mL) was added Pd2dba3 (534mg, 0.58mmol, 0.025eq), PCy3 (660mg, 2.35mmol, O.leq), 2-thiophene boronic acid (3.00g, 23.4mmol, leq), K2C03 (6.48g, 46.9mmol, 2eq), and 4- bromofluorobenzene (5.17mL, 47.0mmol, 2eq). The resultant mixture was stirred overnight at 90C and then allowed to reach room temperature. MgS04 was added to quench water and the mixture was filtered on a pad of Celite using ethyl acetate. The filtrate was concentrated and purified on silica gel chromatography (cyclohexane/ ethyl acetate 100:0 to 95:5) to afford compound 42 (3.84g, 92% yield) as a white solid.

The synthetic route of 460-00-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TFCHEM; DELIENCOURT-GODEFROY, Geraldine; LOPES, Lenaig; WO2012/160218; (2012); A1;,
Bromide – Wikipedia,
bromide – Wiktionary