Month: August 2021

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 17247-58-4 as follows. Recommanded Product: (Bromomethyl)cyclobutane

4e. Preparation of Cyclobutylcarbinylsulfonamide A solution of 12.3 g (83 mmol) of cyclobutylcarbinyl bromide (Aldrich) and 13.7 g (91 mmol) of sodium iodide in 150 mL of acetone was heated to reflux overnight and then cooled to room temperature. The inorganic solids were removed by filtration and the acetone and cyclopropylcarbinyl iodide (8.41 g, 46%) were removed by distillation (ambient temperature and 150 torr at 80 C., respectively). A solution of 4.0 g (21.98 mmol) of cyclobutyl carbinyl iodide in 30 mL of anhydrous diethyl ether cooled to -78 C. was cannulated into a solution of 17 mL (21.98 mmol) of 1.3M sec-butyllithium in cyclohexanes and the solution was stirred for 5 minutes. To this mixture was cannulated a solution of 3.0 g (21.98 mmol) of freshly distilled sulfuryl chloride in 110 mL of hexanes cooled to -78 C., the mixture warmed to room temperature over 1 hour and was then carefully concentrated in vacuo. This mixture was redissolved in diethyl ether, washed once with some ice-cold water, dried (MgSO4), filtered, and concentrated carefully. This mixture was redissolved in 30 mL of THF, added dropwise to 500 mL of saturated NH3 in THF and was allowed to stir overnight. The mixture was concentrated in vacuo to a crude yellow solid and was recrystallized from the minimum amount of dichloromethane in hexanes with 1-2 drops of methanol to provide 1.39 g (42%) of the desired product as a white solid. 1H NMR (CDCl3) delta 1.81-2.03 (m, 4H), 2.14-2.28 (m, 2H), 2.81-2.92 (m, 1H), 3.22 (d, J=7 Hz, 2H), 4.74 (brs, 2H); 13C NMR (CDCl3) delta 19.10, 28.21, 30.64, 60.93. MS m/e 148 (M-H)-.

According to the analysis of related databases, 17247-58-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Bristol-Myers Squibb Company; US2008/119461; (2008); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 1073-39-8, 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. 1073-39-8, name is 3-Bromobicyclo[4.2.0]octa-1,3,5-triene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

20 g (109 mmol) 2-(4-Bromophenyl)-cyclobutyl was dissolved in 150 ml dry THF and cooled to -78 C. 44 ml (109 mmol, 2.5 M solution) of n-Buli was added dropwise and the solution was stirred for one hour at -78 C. 2′- Bromo-biphenyl-2-carboxylic acid (43.6 mmol, 12.7 g) was dissolved in 25 ml THF and added to the n-BuLi solution at -78 C. The reaction mixture was stirred for 1 h at -78 C and then warmed to RT over the weekend. (0187) Ammoniumchloride solution was added to quench the reaction and the mixture was extracted with ethyl acetate. The combined organic phases were dried and the solvent was evaporated in vacuo. The resulting crude product was dissolved in 60 ml dry Toluene and 60 ml Hydrochloric acid (37%) as well as 1 15 ml acetic acid was added. The reaction was stirred at 80 C over night. After cooling down to RT the water was added, the aqueous phase was extracted with toluene and the combined organic phases were washed with water and dried with Na2SO4. The solvent was removed in vacuo. The resulting solid was recrystallized in (0188) Heptane/Toluene. 16 was obtained as a white product with 85% yield (0189) (37.1 mmol, 16.6 g). (0190) 5 I6 (15 g, 33.4 mmol), o-biphenylamine (6.2 g, 36.7 mmol) and Sodium-f- butylate (10.6 g, 1 10 mmol) were dissolved in 200 ml toluene. The mixture was degassed for 15 minutes and subsequently Pd(dppf)CI2 (1 .8 g, 2.2 (0191) mmol) was added. The solution was heated at reflux for 4 hours and then (0192) ^ Q cooled to RT. The mixture was filtered over Alox using toluene as the (0193) solvent. The resulting solid was recrystallized from toluene/heptanes. I7 was obtained as a white solid with a yield of 63% (1 1 .3 g, 21 mmol). (0194) 4.7 g (8.5 mmol) 2,7-dibromo-9,9-dioctyl-fluorene and 10 g (18.6 mmol, 2.2 1 eq) 17 were added to 100 ml Toluene. Subsequently 1 .5 g (1 .7 mmol, 0.2 (0195) eq) Pd2dba3 and 1 .6 g (17 mmol, 2 eq) Sodium-f-butylate were added and the mixture was degassed with argon. After 5 min degassing 3.8 g (1 .7 (0196) mmol, 0.2 eq) tri-f-butylphosphine was added and the reaction was stirred at reflux over the weekend. After cooling to RT the mixture was filtered over (0197) 20 (0198) Celite and subsequently purified via Soxhlet using Toluene as the solvent. (0199) The resulting solid was purified via flash chromatography. 9.7 g (6.6 mmol, 78%) of P8 was obtained.

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

Reference:
Patent; MERCK PATENT GMBH; SCHEIBLE, Katja Maria; ECKES, Fabrice; HEIL, Holger; BURKHART, Beate; JOOSTEN, Dominik; MONTENEGRO, Elvira; (93 pag.)WO2018/65357; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 1347736-74-6,Some common heterocyclic compound, 1347736-74-6, name is 4,7-Dibromo-5-fluoro-2,1,3-benzothiadiazole, molecular formula is C6HBr2FN2S, 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.

(2) a thiadiazole compound of the B-1 (4,7- dibromo-5-fluoro-benzo [c] [1,2,5]; 4,7-dibromo-5-fluorobenzo [c] [1,2,5] thiadiazole) (3.00 g, 9. 6 mmol), A-1Of the compound (3.84 g, 9.58 mmol),Pd2 (dba) 3 (0.174 g, 0.19 mmol), Then triphenylphosphine (triphenylphosphine) (0.202 g, 0.77 mmol) was dissolved in 100 mL of toluene was stirred for 48 hours at 80 .After the reaction, After lowered to normal temperature, into a 2M hydrochloric acid (HCl) and stirred for 1 hour.After the reaction was washed with dichloromethane (dichloromethane) and the solvent removed under reduced pressure. The resulting solid with chloroform (chloroform) to silica column purificationThe compounds of the orange A-2 (1.67 g, yield: 41%) was obtained.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4,7-Dibromo-5-fluoro-2,1,3-benzothiadiazole, its application will become more common.

Reference:
Patent; LG Chem Co.Ltd.; Lim, Bo-Gyu; Bang, Ji-Won; Lee, Jae-Chol; Lee, Ji-Young; Kim, Jin-Seok; Cho, Geun; (37 pag.)KR2015/142609; (2015); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 59907-12-9, A common heterocyclic compound, 59907-12-9, name is 1-Bromo-2-fluoro-3-methylbenzene, molecular formula is C7H6BrF, 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.

1-Bromo-3-bromomethyl-2-fluorobenzene Obtained according to Example E but starting from 1-bromo -2-fluoro- 3-methylbenzene (prepared according to M. S. Newman and R. Kannan, J. Org. Chem., 1976, 41, 3356) and distilling the final product at 20 mm Hg. Yd.: 66% B.p.20 =95-105 C. 1 H N.M.R. (CDCl3): 4.4 (2H, s), 6.6 to 7.6 (3H, m).

The synthetic route of 59907-12-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Lipha, Lyonnaise Industrielle Pharmaceutique; US5489592; (1996); 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. 54962-75-3, name is 3-Bromo-5-(trifluoromethyl)aniline, This compound has unique chemical properties. The synthetic route is as follows., category: bromides-buliding-blocks

Example 7; Preparation of Compound of Formula IVThe compound of formula X (50 g), HOBt (26.5 g)/EDCI (37.5 g) and DMF (500 mL) were loaded into a reactor at 25+/-5 C. After being reacted for 3 h, the compound of formula II (39 g) was added to the reactor. The reaction mixture was stirred at 80 C. for about 18 hours while monitoring for the consumption of active ester by HPLC. After being cooled to 25+/-5 C., the mixture was dropped to a solution of half-saturated aqueous solution of sodium hydrogen carbonate, and the product was precipitated as canary yellow solid.The yield of this step was about 29.0% by weight. The purity of the isolated product was 95% (% on area by HPLC method described in Appendix 1).

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 54962-75-3.

Reference:
Patent; TEVA PHARMACEUTICAL INDUSTRIES LTD.; US2010/16590; (2010); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Some common heterocyclic compound, 328-70-1, name is 1-Bromo-3,5-bis(trifluoromethyl)benzene, molecular formula is C8H3BrF6, 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. Computed Properties of C8H3BrF6

EXAMPLE 3 1-(3,5-Bis(trifluoromethyl)phenyl)ethan-1-one A solution of 3,5-Bis(trifluoromethyl)bromobenzene (29.3 g) in 30 mL of THF was added to a mixture of magnesium granules (5.10 g) in THF (200 mL) heated at reflux (the reaction was initiated with approximately 5 mL of the bromide solution; the remainder was added slowly over 1 h). The mixture was aged for 30 min at reflux, cooled to RT and added over 1 h to a solution of acetic anhydride (40 mL) in THF (40 mL) maintained at -15 C. The resulting dark brown mixture was warmed to 10 C. in a water bath, and water (300 mL) was added. The pH of the vigorously stirred biphasic mixture was adjusted to 8.0 using 50% NaOH. MTBE (300 mL) was added, the layers were separated and the aqueous layer was further extracted with MTBE (3*150 mL). The organic layers were combined and concentrated in vacuo (bath at 30-35 C.; 50-80 torr). The concentrate was then distilled at atmospheric pressure to provide the pure product (20.7 g; 82% yield) with a boiling point of 187-189 C.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 328-70-1, its application will become more common.

Reference:
Patent; McNamara, James M.; Zhao, Matthew M.; US2002/22725; (2002); A1;; ; Patent; Brands, Karel M. Jos; Tsay, Fuh-Rong; Conrad, Karen M.; Zhao, Matthew M.; US2002/52494; (2002); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 21120-91-2, 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. 21120-91-2, name is 7-Bromobicyclo[4.2.0]octa-1,3,5-triene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

7-bromobicyclo[4.2.0]octa- 1 ,3,5-triene (10.0 g,54.6 mmol) and ethylene glycol (100 mE) were added to a250 mE round-bottom flask. The biphasic mixture wascooled to 0 C. followed by the slow addition of solid silver(I) tetrafluoroborate (11.7 g, 60.1 mmol) to maintain a temperature of about 30 C. After addition, the reaction mixture was stirred at 50 C. for 3 hrs. Once cooled down to room temperature, 200 ml water and 400 ml ether were added. The resulting mixture was filtered through celite. The organic layer was washed three times with each 300 ml water and then dried over Na2504 and concentrated to give an oil. The oil was purified by column chromatography on silica gel using 5% ethyl acetate in hexanes (4.66 g). The product had the following characteristics: ?H-NMR (400 MHz, CDC13): oe 7.36-7.27 (m, 1H), 7.27-7.20 (m, 2H), 7.15 (dp, J=7.2, 1.0 Hz, 1H), 5.20-5.03 (m, 1H), 3.90-3.61 (m, 4H), 3.56-3.39 (m, 1H), 3.21- (m, 1H), 2.23-1.98 (br s, 1H). ?3C-NMR (101 MHz, CDC13): oe 145.64, 142.42, 129.49, 127.10, 123.54, 122.70, 76.96, 69.75, 61.91, 38.53

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; Dow Global Technologies LLC; Grigg, Robert David; Spencer, Liam P.; Kramer, John W.; Liu, Chun; Mukhopadhyay, Sukrit; Devore, David D.; Feng, Shaoguang; Feng, Jichang; Zhu, Minrong; (27 pag.)US2018/212180; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 4333-56-6, 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. 4333-56-6, name is Bromocyclopropane belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a stirred solution of bromocyclopropane (Aldrich, 4.2 g, 35 mmol) in tetrahydrofuran (15 mL), magnesium turnings (Aldrich, 0.795 g, 33.1 mmol) were added in three equal portions at room temperature while the reaction was controlled with a water bath so that slight boiling of the solvent was maintained. _

The synthetic route of Bromocyclopropane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Chu, Xin-Jie; Ding, Qingjie; Jiang, Nan; Kim, Kyungjin; Lovey, Allen John; McComas, Warren William; Mullin JR., John Guilfoyle; Tilley, Jefferson Wright; US2004/6058; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 39478-78-9,Some common heterocyclic compound, 39478-78-9, name is 5-Bromo-2-methylaniline, molecular formula is C7H8BrN, 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 1 Preparation of 3-amiotano-4′-chloro-4-methylbiotaphenylTeirakiotas(triotapnenylphosphiotane)palladiotaum (0) (3 7 g, 0 003 mol) and 4-chlorophenylboroniotac acid (20 2 g, 0 13mol) are added to a solution of 5-bromo-2-methylaniotaliotane (20 g, 0 1 mol) in 1 ,2- dimethoxyethane (200 ml) After stirring the reaction mixture for 15 minutes at 2O0C, a solution of 20% aqueous sodium carbonate (300ml) is added to the mixture, and the resulting mixture is heated at reflux for 24 hours. The reaction mixture is cooled to room temperature, diluted with water (600 ml) and extracted using ethyl acetate. The combined organic extracts are dried over anhydrous sodium sulfate, filtered and the filtrate evaporated in vacuo. The residue is further purified by column chromatography on silica gel, eluting with 7% ethyl acetate in hexane to give 3-amino-4′-chloro-4-methylbiphenyl (21.0 g).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-Bromo-2-methylaniline, its application will become more common.

Reference:
Patent; SYNGENTA LIMITED; WO2008/145336; (2008); 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. 1422-54-4, name is 2-Bromo-6-fluorotoluene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 1422-54-4

1-Bromo-3-fluoro-2-methylbenzene (388mg, 2.05mmol), and (4-methoxyphenyl)methanol 5 (0.51 1 mL, 4mmol) were dissolved in DMF (5ml_) in a microwave vessel. Sodium hydride as a 60% dispersion in mineral oil (164mg, 4.0mmol) was added portionwise under a flow of nitrogen over 10min. The reaction vessel was then sealed and heated at 18O0C for 900s. The crude reaction mixture was poured onto 1 :1 wate?brine (6ml_) and DCM (1 OmL). The biphasic mixture was stirred at ambient temperature for 1 h and then the 10 organic and aqueous layers were separated. The combined organics were dried over Na2SO4 and concentrated in vacuo. The crude material was then purified by chromatography on silica gel. Elution with 5:95 ethyl acetate:heptane afforded 1-bromo-3- (4-methoxybenzyloxy)-2-methylbenzene (289mg, 0.9mmol, 46%).

The synthetic route of 1422-54-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; N.V. ORGANON; WO2007/63071; (2007); A1;,
Bromide – Wikipedia,
bromide – Wiktionary