Tag: M.W=100-200

Adding a certain compound to certain chemical reactions, such as: 348-57-2, name is 1-Bromo-2,4-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 348-57-2, Recommanded Product: 1-Bromo-2,4-difluorobenzene

Preparation 131 ,5-dibromo-2,4-difluorobenzeneTo a solution of l-bromo-2,4-difluorobenzene (19.3 mL, 171 mmol) in CH2CI2 (100 mL) was added iron (3.15 g,56 mmol). To this stirred suspension was added a solution of bromine (1 1 mL, 214 mmol) in CH2CI2 (25 mL) drop wise over 30 min. The resulting mixture was stirred at rt overnight. The reaction mixture was slowly poured into saturated aqueous Na2S203 (200 mL), and the resulting mixture was stirred at rt for 30 min. This was extracted with CH2C12 (3 x 80 mL). The combined extracts were washed with brine, dried over MgS04, filtered and concentrated in vacuo to give 1,5-dibromo- 2,4-difluorobenzene (40 g, 86 % yield) as a brown oil. XH NMR (500 MHz,CHLOROFORM-d) delta 7.79 (t, J=7.0 Hz, 1H), 7.00 (t, J=8.2 Hz, 1H).

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-2,4-difluorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; WU, Yong-Jin; WO2012/162334; (2012); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

1003-99-2, name is 2-Bromo-5-fluoroaniline, belongs to bromides-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. name: 2-Bromo-5-fluoroaniline

1-(5-fluoroquinolin-8-yl)piperidin-4-one (Example P, Step 3) is also prepared as shown in the reaction scheme above. To a 500 ml flask equipped with a stirrer, a thermocouple, a condenser and nitrogen inlet were charged 50 g 2-bromo-5-fluoroaniline and 60 g glycerol. The mixture was heated to 60¡ã C. and 55 g nitrobenzene sulfonic acid was charged in portion. The mixture was then heated to 100-110¡ã C., started charge 200 ml 70percent sulfuric acid. After sulfuric acid addition, the mixture was heat to 130¡ã C. and stirred for 3 hours before cooled to room temperature. Water (300 g) was added and a grayish by product was filtered off. The filtrate was slowly added into a 2-L reactor containing a mix of 420 g 50percent NaOH, 420 g of water, 352 g methyl tert-butyl ether. After filtering off small amount solid, the aqueous layer was split off and the organic layer was washed with 10percent NaOH (2.x.100 ml), 20percent NaCl (2.x.200 ml), the solvent was removed, weight 56 g, 89.8percent.

The synthetic route of 1003-99-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Wyeth; US2007/27160; (2007); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 583-70-0, name is 2,4-Dimethylbromobenzene, 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 583-70-0, Safety of 2,4-Dimethylbromobenzene

General procedure: A solution of 4-methoxybromobenzene (2.67 mmol)and cyclopent-2-en-1-one (3.2 mmol) in DMSO was stirred at ambient temperaturefor 10 min under nitrogen, and treated with Na2CO3 (8.01mmol) and tri-tert-butylphosphonium tetrafluoroborate (0.53 mmol).The reaction mixture was degassed with nitrogen for 10 min and treated withPd(PPh3)2Cl2 (0.13 mmol) and X-Phos (0.26mol), and stirred at 100 0C for 12 h. The reaction mixture was cooledto ambient temperature, diluted with water, and extracted with AcOEt (3 x 50ml). The combined organic layers were washed with brine, dried over anhydrousNa2SO4, and evaporated. Flash chromatograph on silica gel(AcOEt:cyclohexane 1:3) provided the Heck coupling product as brown solid (340mg, 68%).

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

Reference:
Article; Gowala, Tarak Nath; Pabba, Jagadish; Tetrahedron Letters; vol. 56; 14; (2015); p. 1801 – 1804;,
Bromide – Wikipedia,
bromide – Wiktionary

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

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 7073-94-1 as follows. Quality Control of 1-Bromo-2-isopropylbenzene

To a solution of 1-bromo-2-isopropylbenzene (388 mg, 298 muL, 1.95 mmol) in dry THF, n-butyllithium (2.5 M in hexanes, 858 muL, 2.14 mmol) was added dropwise at -78 C. After 20 min at -78 C, dimethylformamide (157 mg, 166 muL, 2.14 mmol) was added and the reaction mixture was stirred at -78 C for 20 min and allowed to heat up to -10 C and stirred for 3 h more. Reaction was stopped by adding water (2.5 mL) and extracted with diethyl ether (3 * 100 mL). Combined organic layers were dried over anhydrous MgSO4, filtered, and evaporated, affording 2 with quantitative yield as a colorless oil (277 mg) showing spectral data according to its structure ( Ewing, 1974). It was used with no further purification.

According to the analysis of related databases, 7073-94-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Moreno-Ortega, Ana J.; Martinez-Sanz, Francisco J.; Lajarin-Cuesta, Rocio; De Los Rios, Cristobal; Cano-Abad, Maria F.; Neuropharmacology; vol. 95; (2015); p. 503 – 510;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 6911-87-1, 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. 6911-87-1, name is 4-Bromo-N-methylaniline belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: In air, K2HPO4 (10 mol %, 4.35mg), PMHS (242 mul), amine (0.25 mmol), formic acid (4.6equiv ,43.3mul), 18-crown-6 (20mol %, 13.2mg) 4A MS(10mg) and 2 ml THF were added into a tube equipped with a water condenser. The reaction mixturewas stirred at 80C for 12 hours. The yields of isolated products were reported. The mixture was filtered through a silica gelcolumn with petroleum ether and ethyl acetate as the eluent. The resultant solution was concentrated and purified by silica gelcolumn chromatography to give the corresponding product.

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

Reference:
Article; Huang, Yan; Deng, Wei; Lin, Bo-Lin; Chinese Chemical Letters; (2019);,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 10269-01-9, These common heterocyclic compound, 10269-01-9, name is (3-Bromophenyl)methanamine, 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 3. Preparation of (2R,3R,4R)-2-(6-(3-bromobenzylamino)-2-chloro-9H-purin-9-yl)tetrahydrofuro-3,4-diol After dissolving (2R,3S,4S)-2-(2,6-dichloro-9H-purin-9-yl)tetrahydrofuro-3,4-diol (1 eq.) prepared in the step 2 and 3-bromobenzylamine (1.5 eq.) in ethanol (5 ml) at room temperature, the reaction mixture was stirred at room temperature for 2-3 h. After completion of the reaction, the reaction mixture was concentrated under reduced pressure, and the residue was subjected to silica gel column chromatography using a dichloromethane:methanol mixed solvent (20:1, v/v) as an eluent to obtain the target compound (0.12 g, 82%). mp 181.5-181.7 C.;

Statistics shows that (3-Bromophenyl)methanamine is playing an increasingly important role. we look forward to future research findings about 10269-01-9.

Reference:
Patent; FUTURE MEDICINE CO., LTD.; LEE, Sang Koo; PARK, Chong Woo; KIM, Hea Ok; LEE, Hee Woo; YU, Mi Ra; US2020/16186; (2020); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

32046-62-1, name is 5-Bromo-1H-benzotriazole, belongs to bromides-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. COA of Formula: C6H4BrN3

Example 2008 Compound 2008A (200 mg, 1.02 mmol) was dissolved in 1OmL of CH2CI2 and reacted with DIPEA (0.53 ml, 3.03 mmol), followed by addition of MEMCI (0.15 mL, 1.31 mmol). The reaction mixture was stirred for 16 hours at room temp, then it was added to CH2CI2 and sodium bicarbonate aqueous solution. The organic layers were extracted with CH2CI2, combined and dried over sodium sulfate. The solvent was removed by rotary evaporator to yield compound 2008B (210 mg, 72% yield).

The synthetic route of 32046-62-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SCHERING CORPORATION; WO2007/84451; (2007); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 55289-36-6, 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. 55289-36-6, name is 3-Bromo-2-methylaniline belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of sodium sulfate (61 .1 g, 430 mmol), hydroxylamine hydrochloride (8.96 g, 129 mmol), 2,2,2-trichloro-1 -ethoxyethanol (9.98 g, 51 .6 mmol) and 3-bromo-2- methylaniline (8 g, 43 mmol) in water (300 ml_) was added hydrochloric acid (3.92 ml_, 129 mmol) slowly. This mixture was heated to 90 C for 1 hr. The reaction was cooled, filtered and the solid was washed with water and dried to give 6-bromo-7- methylindoline-2,3-dione (8.6g, 35.8 mmol, 83 % yield) as a brown solid.

The synthetic route of 3-Bromo-2-methylaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; JIN, Qi; POHLHAUS, Denise Teotico; SPLETSTOSER, Jared; (320 pag.)WO2017/98440; (2017); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 108-85-0, 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. 108-85-0, name is Bromocyclohexane belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: Alkyne (1mmol), sodium azide (1.1mmol), organic halide (1mmol), and water (3mL) were placed together in a 10mL round-bottom flask. PS-C22-CuI (40mg, containing 0.6mol% of Cu) was then added to the above solution. The suspension was magnetically stirred for 10h at room temperature. After completion of the reaction as followed by TLC, EtOAc (5mL) was added to the mixture, filtered, and washed with water (2¡Á3mL) and EtOAc (2¡Á3mL). The organic phase was separated, dried (MgSO4), and concentrated in vacuum to give the crude product that was further purified by recrystallization with ethanol/water (3:1 v/v). In the case of triazole 5h, after completion of the reaction, water was evaporated and EtOAc (5mL) was added. The mixture was filtered to separate the catalyst and the filtrate was concentrated under vacuum to obtain the desired product, which was almost pure.

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, Bromocyclohexane, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Movassagh, Barahman; Rezaei, Nasrin; Tetrahedron; vol. 70; 46; (2014); p. 8885 – 8892;,
Bromide – Wikipedia,
bromide – Wiktionary