Tag: M.W=100-200

Reference of 1422-53-3, 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. 1422-53-3, name is 2-Bromo-4-fluorotoluene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

2-bromo-4-fluorotoluene 25g (132.3mmol, 1.0eq), AIBN 521mg (3.2mmol, 0.024eq),Co(OAc) 2·4H2O 1.6 g (6.5 mmol, 0.049 eq), NaBr 449 mg (4.4 mmol, 0.033 eq), dissolved in HOAc 250 mL (10V)Stir the whole solution, increase the temperature of the outer bath of the reaction coil to 130 C, adjust the coil pressure to 1.2 MPa with oxygen, and start the materialing. The system residence time is 1.5 h and the oxygen is 3 to 5 eq.The system was directly pumped into 375 mL of purified water, and the pH of the system was adjusted to 12-14 with NaOH solids.The aqueous phase was extracted twice with 125 mL MTBE, and the aqueous phase was adjusted to pH 1 with concentrated HCl.A large amount of solid was precipitated, and 11.8 g of the target product was obtained by filtration, yield 41%.

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

Reference:
Patent; Jilinkai Laiying Pharmaceutical And Chemical Co., Ltd.; Hong Hao; Zhang Enxuan; Lu Jiangping; Liu Zhiqing; Li Chao; Tan Yang; (16 pag.)CN110218150; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

583-70-0, name is 2,4-Dimethylbromobenzene, 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. Formula: C8H9Br

Under a nitrogen atmosphere, cuprous iodide (3.0 mol%, 0.7 mg), sodium iodide (1.0 equiv., 18.7 mg) and magnets were added to a previously baked 10 mL glass pressure tube. Dioxane (0.2 mL), 2,4-dimethylbromobenzene (0.125 mmol, 1.0 equiv., 23.2 mg) and N,N’-dimethylethylenediamine (10.0 mol%, 1.1 mg) were then added. ). After the addition was completed, the glass pressure tube was placed in a metal module that had been preheated to 100 deg C and stirred for 10 hours. After cooling to room temperature, copper powder (20 mol%, 1.6 mg), aluminum chloride (3 mol%, 0.5 mg), N-methylpyrrolidone (0.5 mL) and polymethylhydrogensiloxane (3.0 equiv) were added under a nitrogen atmosphere. ., 83.4mg). The tube was purged of air and charged with carbon dioxide (5.0 equiv., 15 mL) and ammonia gas (5.0 equiv., 15 mL). After the addition was completed, the reactor was placed in a metal module preheated to 160 deg C and stirred for 10 hours. After the reaction was completed, the reaction system was cooled to room temperature and pressure was slowly released. Using dodecane as an internal standard, the yield of the gas chromatogram was determined to be 78%.

The synthetic route of 583-70-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Chinese Academy Of Sciences Lanzhou Chemical Physics Institute Suzhou Institute; Li Yuehui; Wang Hua; Dong Yanan; Ke Lisitian·shanduofu; (20 pag.)CN108017557; (2018); A;,
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. 586-61-8, name is 1-Bromo-4-isopropylbenzene, This compound has unique chemical properties. The synthetic route is as follows., name: 1-Bromo-4-isopropylbenzene

Compound 1-3 (5.28 g, 10 mmol) and 4-isopropyl-bromobenzene (4 g, 20 mmol)Add in a three-necked flask and stir to dissolve with 100 ml of anhydrous toluene.Nitrogen protection followed by Pd(dba)2 (575mg, 1mmol)And sodium tert-butoxide (1.93 g, 20 mmol),Then, a solution of 10% of tri-tert-butylphosphine toluene (4.5 ml) was added, and the reaction solution was stirred and refluxed overnight.After the reaction was completed, it was cooled, and the reaction liquid was washed three times with 100 ml of water.The organic phase was dried over anhydrous sodium sulfate and then evaporated to remove solvent.The residue was purified by DCM/PE (1:15).Obtained white solid compound Cl(4.95 g, yield 56%).

According to the analysis of related databases, 586-61-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Guangzhou Huarui Optoelectric Materials Co., Ltd.; Yang Xi; Pan Junyou; Chen Jia; (38 pag.)CN109608342; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 2695-48-9, name is 8-Bromo-1-octene, 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 2695-48-9, Formula: C8H15Br

Intermediate 104b tert-butyl 4-hydroxydodec-11-enoate Magnesium turnings (307 mg, 12.64 mmol) was weighed into a pre-dried flask and dried in an oven at 120 C for 2 hours. The flask was removed from the oven, sealed, and cooled to ambient temperature. To the flask, 6 ml_ of anhydrous THF and one particle of iodine was added, followed by addition of 8-bromooct-1-ene (1.570 g, 8.22 mmol). A condenser was added to the flask, and the whole system was exhanged with N2 and protected under N2 ballon. The reaction was heated with a heating until the brown color from the iodine disipated. The reaction was heated at reflux until most of magnesium was consumed (about 1.5 hr), then cooled to room temperature. To a solution of Intermediate 104a (1.0g, 6.32mmol) in 25ml THF cooled in a dry-ice acetone bath, the freshly prepared Grignard reagent was added dropwise. The reaction was stirred for 1 h, then warmed to ambient temperature. The reaction was quenched with sat. aq. NaHC03, and extracted with ethyl acetate. The combined organics were dried over sodium sulfate and filtered. The filtrate was concentrated under reduced pressure and purfied on silica gel with 10% ethyl acetate / heptane to afford the desired product (890mg, 60%). 1H NMR (400 MHz, CDCI3) delta = 5.61-5.85 (m, 1 H), 4.80-4.98 (m, 2H), 3.48-3.62 (m, 1 H), 2.26-2.36 (t, J=7.5Hz, 2H), 1.50- 1.78 (m, 4H), 1.35-1.44 (m, 19H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 8-Bromo-1-octene, and friends who are interested can also refer to it.

Reference:
Patent; NOVARTIS AG; BRITO, Luis; CHEN, Delai; GAMBER, Gabriel Grant; GEALL, Andrew; LOVE, Kevin; ZABAWA, Thomas; ZECRI, Frederic; WO2015/95346; (2015); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 17247-58-4, name is (Bromomethyl)cyclobutane belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. name: (Bromomethyl)cyclobutane

A stirred solution of the ketimime 1a’ (50 g, 187.1 mmol, available from Aldrich Chemical Company, Milwaukee, Wis.) under N2 in dry THF (400 mL) was cooled to -78 C. and treated with 1 M solution of K-tBuO (220 mL, 1.15 equiv.) in THF. The reaction mixture was warmed to 0 C. and stirred for 1 h and treated with bromomethylcyclobutane (28 mL, 249 mmol). The reaction mixture was stirred at room temperature for 48 h and concentrated in vacuo. The residue was dissolved in Et2O (300 mL) and treated with aq. HCl (2 M, 300 mL) The resulting solution was stirred at room temperature for 5 h and extracted with Et2O (1 L). The aqueous layer was made basic to pH12-14 with aq. NaOH (50%) and extracted with CH2Cl2 (3×300 mL). The combined organic layers were dried (MgSO4), filtered, and concentrated to give pure amine (1b’, 18 g) as a colorless oil.

The synthetic route of 17247-58-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Schering Corporation; US2006/276406; (2006); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 4117-09-3, name is 7-Bromo-1-heptene, 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 4117-09-3, Recommanded Product: 7-Bromo-1-heptene

Production Example 9To a mixture of 0.20 g of N- (3-hydroxyphenyl) methyl-benzothiazole-6-carboxamide, 0.16 g of 7-bromo-l-heptene and 5 ml of DMF- was added 0.26 g of cesium carbonate, and the mixture was stirred at room temperature for 4 hours. To the reaction mixture was added water, and the generated solid was collected by filtration. The solid was washed sequentially with a sodium hydroxide aqueous solution, water and hexane, and 0.12 g of N- (3- ( 6-heptenyloxy) phenyl) methyl-benzothiazole-6-carboxami de (hereinafter, referred to as the compound (9) of the present invention) was obtained.The compound (9) of the present invention 1H-NMR (CDCl3) delta: 9.11 (IH, s) , 8.50 (IH, d, J = 1.7 Hz) , 8.16 (IH, d, J = 8.5 Hz) , 7.88 (IH, dd, J = 8.5, 1.7 Hz) , 7.27 (IH, t, J = 7.9 Hz) , 6.95-6.91 (2H, m) , 6.84 (IH, dd, J = 8.3, 2.4Hz) , 6.50 (IH, s) , 5.86-5.76 (IH, m) , 5.00 (IH, dq, J = 17.1,1.7 Hz) , 4.94 (IH, dd, J = 10.2, 2.0 Hz) , 4.66 (2H, d, J = 5.6Hz) , 3.95 (2H, t, J = 6.5 Hz) , 2.08 (2H, d, J = 6.8 Hz) , 1.82-1.75 (2H, m) , 1.52-1.42 (4H, m) .

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; SUMITOMO CHEMICAL COMPANY, LIMITED; WO2009/157528; (2009); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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, HPLC of Formula: C6H3BrF2

To a 0 C. mixture of 1-bromo-2,4-difluorobenzene (20.0 g; 11.7 mL; 0.100 mol) and H2SO4 (76.8 mL) was added HNO3 (68.0 mL) over 45 min at such a rate that the internal temperature was < 7 C. The resulting mixture was stirred for 1 h at 0 C., poured into ice water (400 mL), stirred vigorously for 2-3 min and extracted with CH2Cl2 (400 mL). The CH2Cl2 extract was washed with brine (1?500 mL), dried over Na2SO4, filtered and evaporated to give the product as a yellow oil (23.5 g, 95percent). 1H NMR (300 MHz, CDCl3) ? 7.14 (ddd, J=0.3, 7.8, 9.9 Hz, 1H), 8.39 (t, J=7.2 Hz, 1H). At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-2,4-difluorobenzene, and friends who are interested can also refer to it. Reference:
Patent; Synaptic Pharmaceutical Corporation; US2005/154020; (2005); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 399-94-0, These common heterocyclic compound, 399-94-0, name is 1-Bromo-2,5-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.

A solution of tert-butyl pyrrolidine- 1-carboxylate (20 g, 116.8 mmol) and (- )sparteine (32.9, 140 mmol) in MTBE (360 mL) was cooled to -78 0C, and sec-BuLi (10OmL, 140 mmol, 1.4 M in cyclohexane) was introduced drop-wise via cannula, keeping the internal temperature under -70 0C. The resulting solution was stirred for 3 hours at -78 0C, followed by addition of a solution of ZnCl2 (93.4 mL, 93.4 mmol, IM in Et2O) drop-wise with rapid stirring, keeping the internal temperature below -65 0C. The resulting light suspension was stirred at -78 0C for 30 minutes and then warmed to ambient temperature. The resulting mixture was charged with 2-bromo-l,4-difluorobenzene (14.5 mL, 128 mmol), followed by Pd(OAc)2 (1.31 g, 5.8mmol) and ^-Bu3P-HBF4 (2.03 g, 7.0 mmol) in one portion. After stirring overnight at ambient temperature, 10.5 mL Of NH4OH solution was added and the reaction was stirred for another hour. The resulting slurry was filtered through CELITE and washed with Et2O (1 L). The filtrate was washed with HCl (0.5 L, IM aq.) and brine. The organic layer was filtered and concentrated, and the crude product was purified by silica column chromatography, eluting with 5-10% EtO Ac/hex anes to give product (R)-tert-butyl 2- (2,5-difluorophenyl)pyrrolidine- 1-carboxylate as yellow oil (23.9 g, 72% yield).

The synthetic route of 399-94-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ARRAY BIOPHARMA INC.; ANDREWS, Steven, W.; HAAS, Julia; JIANG, Yutong; ZHANG, Gan; WO2010/33941; (2010); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 3814-30-0, name is (Bromomethyl)cyclopentane, 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 3814-30-0, Computed Properties of C6H11Br

To a solution of 3-(tetrahydro-2H-pyran-4-yI)imidazo[1 ,5-a]pyrazin-8(7H)-one (400 mg, 1 .82 mmol) in anhydrous DMF (5 mL) was added K2003 (503 mg, 3.64mmol) and (bromomethyl)cyclopentane (445 mg, 2.73 mmol). The reaction mixture was stirred at 6000 for 16 hours. The mixture was filtered and the filtrate was purified bypreparative LC-MS to afford 7-(cyclopentylmethyl)-3-(tetrahydro-2H-pyran-4-yl)i midazo[1 ,5- a]pyrazin-8(7H)-one 290 mg (53%).1H NMR (DMSO-d6, 400 Mhz): 7.62 (s, 1H), 7.49 (d, J= 6.0 Hz, 1H), 6.90 (d, J= 6.0 Hz,1H), 3.91-3.88 (m, 2H), 3.69 (d, J= 7.6Hz, 2H), 3.48-3.43 (m, 2H), 3.42-3.31 (m, 1H), 2.27-2.24 (m, 1H), 1.78-1.73 (m, 4H), 1.58-1.44 (m, 6H), 1.21-1.20 (m, 2H).LC-MS: (mlz) 302.2 (MH) tR (minutes, method 3) = 2.29 minutes

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, (Bromomethyl)cyclopentane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; H. LUNDBECK A/S; KEHLER, Jan; RASMUSSEN, Lars, Kyhn; LANGGARD, Morten; JESSING, Mikkel; VITAL, Paulo, Jorge, Vieira; JUHL, Karsten; (159 pag.)WO2016/174188; (2016); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 1003-99-2, 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. 1003-99-2 name is 2-Bromo-5-fluoroaniline, 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.

2-1 (200 g, 1053 mmol) and diethyl ethoxymethylenemalonate (228 g, 1053 mmol) were combined neat and heated to 120 “C. After 2 h, the reaction was poured hot into 2 L of methanol. The resulting mixture was cooled to 10 C and filtered, washing with methanol. The product was dried on the filter under N2, yielding 320 g (84%) of 2-2 in two crops. MS (Electrospray): m/z 315.9 (MH+-CO2)-

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

Reference:
Patent; MERCK & CO., INC.; WO2008/2621; (2008); A2;,
Bromide – Wikipedia,
bromide – Wiktionary