Tag: M.W=300-400

Reference of 10016-52-1, The chemical industry reduces the impact on the environment during synthesis 10016-52-1, name is 2,8-Dibromodibenzo[b,d]furan, I believe this compound will play a more active role in future production and life.

In a 25 ml four-necked flask, 0.52 g (2.0 mmol) of 4-phenylaminodibenzofuran, 0.33 g (1.0 mmol) of 2,8-dibromodibenzofuran, 500 mg (5.2 mmol) of sodium t-butoxide, 10 ml of dehydrated toluene In addition, nitrogen bubbling was performed for 1 hour. after that,Pd2 (dba) 392 mg (0.10 mmol),After adding 58 mg (0.20 mmol) of tri-t-butylphosphonium tetrafluoroborate, the mixture was heated under reflux for 12 hours while stirring under a nitrogen stream. The formation of the desired product was confirmed by TLC and MS. The reaction solution was cooled to room temperature, and the organic layer was extracted with toluene, washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated to obtain a brown viscous product. The resulting gum was dissolved in 5 ml of toluene and loaded onto the column. The crude product was directly purified by silica gel column chromatography (developing solvent: toluene / hexane = 1/4) to obtain 0.51 g of the target product HTM5 in a yield of 75%.

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, 2,8-Dibromodibenzo[b,d]furan, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; National University Corporation Yamagata University; Sasabe, Hisahiro; Kido, Junji; Kamata, Takahiro; (21 pag.)JP2019/26556; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 2789-89-1, These common heterocyclic compound, 2789-89-1, name is 1,2-Bis(4-bromophenyl)ethyne, 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: Alkyne (0.5 mmol, 1 equiv.), primary alcohol (0.5 mmol, 1 equiv.), I2 (1 mmol, 253.8 mg, 2 equiv.) and DMSO (2 mL) were mixed in a round bottom flask and heated at 130 C for 24 h. Thereafter, ammonium acetate (5 mmol, 385.4 mg, 10 equiv.) and EtOH (2 mL) was added to the mixture and heated at 100 C for 2 h. After cooling, a solution of 1% Na2S2O3 was added dropwise to the mixture to form a precipitate which was filtered and dried. The crude product was recrystallized from EtOH to afford spectroscopically pure imidazole 3.

The synthetic route of 2789-89-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Jeena, Vineet; Naidoo, Shivani; Tetrahedron; (2020);,
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. 52997-43-0, name is 7-(Bromomethyl)pentadecane, A new synthetic method of this compound is introduced below., SDS of cas: 52997-43-0

General procedure: General procedure for the synthesis of a1-a6: To a solution of indoline-2,3-diones (10 mmol) in DMF (40 mL) was added K2CO3(15 mmol, 2.073 g) and 7-(bromomethyl)pentadecane (11 mmol,3.358 g) under nitrogen. The mixture was stirred at 70 C and monitoredby TLC. After the reaction completed, water was added, andextracted with EtOAc. The organic layer was combined and dried withMgSO4. After evaporation of the solvent, the residue was purified bycolumn chromatograph (eluent: Petroleum/EtOAc=20:1) to give thetarget compound.

The synthetic route of 52997-43-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Hu, Qian; Jiang, Hua; Cui, Zhihua; Chen, Weiguo; Dyes and Pigments; vol. 173; (2020);,
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. 43204-63-3, name is Bis(2-Bromoethyl)amine hydrobromide, A new synthetic method of this compound is introduced below., HPLC of Formula: C4H10Br3N

Step 4: 4,5-Difluoro-2-(piperazin-1-yl)benzenesulfonamide A mixture of 2-amino-4,5-difluoro-benzenesulfonamide (1.04 g, 5.00 mmol), 2-bromo-N-(2-bromoethyl)ethanamine hydrobromide (15.59 g, 50.00 mmol) and n-butyl alcohol (50.00 mL) was stirred at 120 C. for 40 h. The reaction mixture was filtered and the filtrate was concentrated in vacuo. The residue was purified via preparative HPLC to afford 4,5-difluoro-2-piperazin-1-yl-benzenesulfonamide (400.00 mg, 1.15 mmol, 23% yield, 80% purity) as a white solid. MS (EI+, m/z): 278.1 [M+H]+.

The synthetic route of 43204-63-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Navitor Pharmaceuticals, Inc.; O’Neill, David John; Saiah, Eddine; Kang, Seong Woo Anthony; Brearley, Andrew; Bentley, Jonathan; (519 pag.)US2018/127370; (2018); 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. 18648-66-3, name is 2-(4-Bromophenyl)-1,1-diphenylethylene, A new synthetic method of this compound is introduced below., HPLC of Formula: C20H15Br

P-aminobenzeneboronic acid hydrochloride was added1000ml three-necked flask, add 800ml tetrahydrofuran, then add 2mol / L potassium carbonate solution 168ml, magnetic stirring and argon, oil bath heated to 70 , adding 0.1g tetraphenylphenylphosphine palladium, reflux reaction 24h, The reaction product was spin-dried and the product was spin-dried to dry the powder and dried in vacuo at 60 C for 24 h to give the white intermediate TriP-NH2 in 86% yield.

The synthetic route of 18648-66-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sun Yat-sen University; Zhang, Yi; Liu, Yiwu; Xu, Jiarui; Wu, Xinhui; Shi, Jie; Liu, Siwei; Chi, Zhenguo; (20 pag.)CN104341311; (2016); B;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 2789-89-1, name is 1,2-Bis(4-bromophenyl)ethyne, 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. Recommanded Product: 1,2-Bis(4-bromophenyl)ethyne

Example 125 Preparation of N-phenyl-3,4-di(p-bromophenyl)-1-phenyl-1,2-dihydrobenz[c-1,2]azaphosphinine 1-oxide N-phenyl-3,4-di(p-bromophenyl)-1-phenyl-1,2-dihydrobenz[c-1,2]azaphosphinine 1-oxide (81.9 mg, 87%) as a target compound was obtained under the condition of 110 for 30 hours, by the same reaction as the Example 118 above, except for using 1,2-bis(4-bromophenyl)ethyne (100.8 mg, 0.3 mmol) instead of using 3-hexyne of the Example 118 above. 1H NMR (400 MHz, CDCl3) delta 7.68 (dd, J=7.1 Hz, 12.9 Hz, 2H), 7.51 (dd, J=7.4 Hz, 14.2 Hz, 1H), 7.43 (t, J=7.7 Hz, 1H), 7.38-7.35 (m, 3H), 7.31-7.25 (m, 3H), 7.11-7.06 (m, 3H), 7.01-7.00 (m, 4H), 6.88 (t, J=7.8 Hz, 4H), 6.81 (t, J=7.2 Hz, 1H)

The synthetic route of 1,2-Bis(4-bromophenyl)ethyne has been constantly updated, and we look forward to future research findings.

Reference:
Patent; KNU-INDUSTRY COOPERATION FOUNDATION; Lee, Phil Ho; Park, Young Chul; Jeon, In Cheol; Seo, Jung Min; Seo, Bo Ram; US2015/344506; (2015); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 18648-66-3, name is 2-(4-Bromophenyl)-1,1-diphenylethylene, 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 18648-66-3, Safety of 2-(4-Bromophenyl)-1,1-diphenylethylene

theTriphenylethylene bromide (3.35g,10.0mmol) dissolved in 20ml of tetrahydrofuran,cool down to -78 C, slowly drop wise added 2.5M n-butyllithium solution(4.0ml,10.0ml). After the addition was complete for 2 h, N, N-dimethylformamide(1.46g,20.0ml)was added, naturally heated to room temperature and kept thereaction for 24 h. The reaction was terminated, extraction was carried out withwater,after organic phase was dried over anhydrous sodium sulfate and dried invacuo on a rotary evaporator to give the crude product. The product waspurified by silica gel column chromatography; the eluent was a mixed solvent ofdichloromethane and n-hexane with volume ratio of 3:1. Pure product as a whitesolid, 3.3 g (yield 81%).

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

Reference:
Patent; Sun Yat-sen University; Ma, ChunPing; Chi, ZhenGuo; Zhou, Xie; Zhang, Yi; Liu, SiWei; Xu, JiaRui; (14 pag.)CN103804318; (2016); B;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 2789-89-1, These common heterocyclic compound, 2789-89-1, name is 1,2-Bis(4-bromophenyl)ethyne, 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.

Example 45 Preparation of 3,4-Bis(4-bromophenyl)-1-phenyl-1H-2,1-benzoxaphosphinine 1-oxide 3,4-Bis(4-bromophenyl)-1-phenyl-1H-2,1-benzoxaphosphinine 1-oxide (47.2 mg, 57%) as a target product was obtained under the condition of 90 C. for 30 hours, by the same reaction as the Example 1 above, except for using diphenylphosphinic acid (32.7 mg, 0.15 mmol) instead of using phenylphosphonic monoethyl ester of the Example 1 above, and using 1,2-bis(4-bromophenyl)ethyne (75.6 mg, 0.23 mmol) instead of using diphenylacetylene of the Example 1 above. 1H NMR (400 MHz, CDCl3) delta 7.94-7.89 (m, 2H), 7.66-7.51 (m, 6H), 7.47 (tt, J=7.7, 1.2 Hz, 1H), 7.39-7.34 (m, 1H), 7.28 (app d, J=8.7 Hz, 2H), 7.15 (d, J=8.2 Hz, 2H), 7.09 (app d, J=8.7 Hz, 2H), 7.01 (dd, J=8.0, 4.7 Hz, 1H).

The synthetic route of 2789-89-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; KNU-INDUSTRY COOPERATION FOUNDATION; Lee, Phil Ho; Park, Young Chul; Jeon, In Cheol; Seo, Jung Min; Seo, Bo Ram; US2015/344506; (2015); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Some common heterocyclic compound, 20191-76-8, name is 2,4-Dibromonaphthalen-1-amine, molecular formula is C10H7Br2N, 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. category: bromides-buliding-blocks

52.0 g (172 mmol) of 48-4, 12.1 g (17 mmol) of Pd (dppf) Cl2,63.2 g (518 mmol) of phenylboronic acid, 119.4 g (863 mmol) of K2CO3,The EtOH / H2O mixture was refluxed at 80C for 6 hours. After the temperature was lowered and the mixture was extracted with MC / H2O, the organic layer was dried over MgSO4.After concentration, the product was purified by column chromatography (SiO2, hexane: MC = 1: 2)To thereby obtain objective compound 48-3 (42.0 g, 82%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 20191-76-8, its application will become more common.

Reference:
Patent; HEESUNG MAT LTD; Hui Sanctum Jae Co., Ltd.; JUNG YU JUN; Jeong Yu-jun; DONG GWANG IL; Dong Gwang-il; KIM YONG WOO; Kim Yong-u; CHOI JIN SEOK; Choi Jin-seok; CHOI DAE HYUK; Choi Dae-hyeok; LEE JOO DONG; Lee Ju-dong; (34 pag.)KR2018/72058; (2018); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 10016-52-1,Some common heterocyclic compound, 10016-52-1, name is 2,8-Dibromodibenzo[b,d]furan, molecular formula is C12H6Br2O, 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.

To a two-necked flask were added A-1-1 (2.5 g), B-1 (3.6 g) And sodium tert-butoxide (4.4 g) was added thereto. The flask was filled with di-gassed toluene (46 mL) and heated to 100 C. Pd [P (t-Bu) 3] 2 (200 mg), Pd And the mixture was stirred at the same temperature for 17 hours. Diluted with DCM (100 mL) and filtered through SiO2. The filtered solution was depressurized to remove the solvent, and the residue was dissolved in THF in EA and then recrystallized to obtain A-1 (final) (1.5 g).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,8-Dibromodibenzo[b,d]furan, its application will become more common.

Reference:
Patent; LG Chem, Ltd.; Lee Chung-hwan; Bae Jae-sun; Lee Jae-cheol; Kim Hwa-gyeong; Shin Ji-yeon; (37 pag.)KR2018/92782; (2018); A;,
Bromide – Wikipedia,
bromide – Wiktionary