Tag: M.W=300-400

52997-43-0, 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 52997-43-0 as follows.

Under nitrogen protection, nitrogen is protected. The intermediate product 1, 2 – bis (4 -hydroxyphenyl) ethane -1, 2 – diketone (2g, 8.26 mmol), potassium carbonate (2.4g, 0.2 mmol), tetrabutylammonium bromide (1.33g, 4.13 mmol) were dissolved in N 70 ml) solutions, followed by 60 C stirring 1h, followed by 7 – (bromomethyl) pentadecane (4.04g, 13.2 mmol), 120 C and refluxing 24h out unitunit_ type. After completion of the reaction, the reaction was completed. The reaction solution was cooled to room temperature, and saturated 200 ml brine and dichloromethane were added thereto to extract, and the organic phase, dried over anhydrous magnesium sulfate, concentrated, and then subjected to column chromatography separation and purification. The eluate containing the objective compound was collected by column 300 – 400 silica gel as a 1:3 stationary phase, eluting, with a dichloromethane/petroleum ether volume ratio timetime mixture and dried, yielding a yellow powdery intermediate product 1, 2 – bis (4 – (hexadecyloxy) phenyl) ethane -1, was obtained. 2 – Diketone 3.05g, yield=unitz 45.4%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 52997-43-0, and friends who are interested can also refer to it.

Reference:
Patent; Zhejiang University of Technology; Lv Xiaojing; Bi Qian; Ouyang Mi; Qian Liang; Xu Xinjia; Zha Lixia; (13 pag.)CN110066287; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

615-54-3, 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. 615-54-3, name is 1,2,4-Tribromobenzene, A new synthetic method of this compound is introduced below.

Under an argon stream, 1.50 g (6.02 mmol) of 4- (2-quinolyl) phenylboronic acid,542 mg (1.72 mmol) of 1,2,4-tribromobenzene,159 mg (0.138 mmol) of tetrakis (triphenylphosphine) palladium,And 7.74 mL (7.74 mmol) of 1 M potassium carbonate aqueous solution were dissolved in 60 mL of dioxane,And the mixture was heated and stirred at 100 C.After cooling to room temperature, 500 mL of pure water was added and the mixture was separated and extracted with chloroform.After distilling off the solvent under reduced pressure, the obtained crude product was recrystallized twice using toluene as a solvent,Objective4,4 ” – di (2-quinolyl) -4 ‘- [4- (2-quinolyl) phenyl] -1,1’: 2 ‘, 1 “Of a white solid (yield 680 mg, yield 57.5%).

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; TOSOH CORPORATION; FUJITA, KANA; ARAI, NOBUMICHI; NOMURA, KEISUKE; IIDA, TAKASHI; TANAKA, TSUYOSHI; (76 pag.)JP6264877; (2018); B2;,
Bromide – Wikipedia,
bromide – Wiktionary

955959-84-9, These common heterocyclic compound, 955959-84-9, name is 4-(4-Bromophenyl)dibenzo[b,d]furan, 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.

In a 250 ml three-necked flask, 0.012 mol of the raw material 1-1, 0.010 mol of the raw material II-1, and 150 ml of toluene were added and stirred under a nitrogen atmosphere.Then add 5¡Á10-5 mol Pd2(dba)3, 5¡Á10-5 mol P(t-Bu)3, 0.03 mol sodium tert-butoxide, heated to 105 C, refluxed for 24 hours, sampling the plate, showing no bromine remaining, the reaction is complete; naturally cooled to room temperature, filtered, and the filtrate is rotary evaporated to no fraction, and passed through a neutral silica gel column to obtain the desired product intermediate B-1; HPLC purity 99.93%, yield 77.3%;

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 955959-84-9.

Reference:
Patent; Jiangsu March Optoelectric Technology Co., Ltd.; Tang Dandan; Li Chong; Zhang Zhaochao; Ye Zhonghua; (71 pag.)CN109761967; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 955959-84-9, name is 4-(4-Bromophenyl)dibenzo[b,d]furan, 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 955959-84-9, 955959-84-9

6.3 g (15.4 mmol) of N-phenyl-3,3-bicarbazole, 5.0 g (15.4 mmol) of 4-(4-bromophenyl)dibenzo[b,d]furan, 3.0 g (30.7 mmol) of sodium t-butoxide, 0.9 g (1.5 mmol) of tris(dibenzylideneacetone)dipalladium, and 1.2 mL of tri t-butylphosphine (50% in toluene) were mixed with 100 mL of xylene in a 250 mL round flask, and the mixture was heated and refluxed under a nitrogen flow for 15 hours. The obtained mixture was added to 300 mL of methanol, and a solid crystallized therein was filtered, dissolved in dichlorobenzene, filtered with silica gel/Celite, and after removing an appropriate amount of an organic solvent, recrystallized with methanol to obtain Compound B-78 (7.3 g, a yield of 73%). (0183) calcd. C48H30N2O: C, 88.59; H, 4.65; N, 4.30; O, 2.46. found: C, 88.56; H, 4.62; N, 4.20; 0, 2.43.

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-(4-Bromophenyl)dibenzo[b,d]furan, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SAMSUNG SDI CO., LTD.; JUNG, Ho Kuk; LUI, Jinhyun; KIM, Dong-Yeong; JANG, Kipo; HUH, Dal-Ho; YU, Eun Sun; JUNG, Sung-Hyun; (75 pag.)US2019/280211; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

52997-43-0, Adding some certain compound to certain chemical reactions, such as: 52997-43-0, name is 7-(Bromomethyl)pentadecane, 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 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. 1-(2-Hexyldecyl)indoline-2,3-dione (a1) Orange oil, 3.46 g, 93%.FT-IR (KBr) nu=1743 and 1612 cm-1 (C]O). 1H NMR (400 MHz,CDCl3) delta 7.60-7.55 (m, 2H), 7.10 (dd, J1=7.2 Hz, J2=7.6 Hz, 1H),6.86 (d, J=8.0 Hz, 1H), 3.59 (d, J=7.2 Hz, 2H), 1.86-1.81 (m, 1H),1.34-1.23 (m, 24H), 0.88-0.83 (m, 6H); 13C NMR (100 MHz, CDCl3) delta183.28, 158.19, 151.21, 138.20, 124.90, 123.32, 117.29, 110.30,44.42, 35.78, 31.64, 31.54, 31.27, 29.73, 29.40, 29.29, 29.06, 26.12,26.09, 22.44, 22.41, 13.88, 13.84. ESI-MS(100%, negative) m/z=371.2 (M-).

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 52997-43-0.

Reference:
Article; Hu, Qian; Jiang, Hua; Cui, Zhihua; Chen, Weiguo; Dyes and Pigments; vol. 173; (2020);,
Bromide – Wikipedia,
bromide – Wiktionary

955959-84-9, The chemical industry reduces the impact on the environment during synthesis 955959-84-9, name is 4-(4-Bromophenyl)dibenzo[b,d]furan, I believe this compound will play a more active role in future production and life.

The specific synthetic route of the compound is now provided:250ml of four bottles, in the atmosphere of nitrogen,0.01 mol of 2- (4-bromophenyl) -dibenzofuran, 0.025 mol of acridine,0.03 mol sodium tert-butoxide, 1 x 10-4 mol Pd2 (dba) 3, 1 x 10-4 mol tri-tert-butylphosphine,150ml toluene, heated reflux 24 hours, sampling point plate, the reaction is complete, natural cooling, filtration,The filtrate was steamed and passed through a silica gel column to give the target product with 99.0percent purity and 69.00percent yield.

The chemical industry reduces the impact on the environment during synthesis 4-(4-Bromophenyl)dibenzo[b,d]furan. I believe this compound will play a more active role in future production and life.

Reference:
Patent; CECEP Wanrun Co., Ltd.; Li Chong; Xu Kai; Zhang Zhaochao; (37 pag.)CN107056758; (2017); A;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 52997-43-0, name is 7-(Bromomethyl)pentadecane, 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. 52997-43-0

In an oven-dried two-neck round-bottom flask, Cs2CO3 (15.6 g, 48.0 mmol) was dissolved in anhydrous DMF (100 mL) and the mixture was heated to reflux under a nitrogen atmosphere. After 15 min, phenol (3.76 g, 40.0 mmol), and, after an additional 40 min, 7-(bromomethyl)pentadecane (S1) (202 g, 66.3 mmol) were added. The progress of the reaction was monitored via TLC and after complete conversion of phenol, the reaction mixture was cooled to r.t. and the solvent was removed under reduced pressure. The residue was taken up in CH2Cl2, filtered, and washed with water and brine. Purification by column chromatography (silica gel, hexanes) afforded the title compound as a colorless oil. Yield: 10.8 g (33.9 mmol, 85%). 1H NMR (400 MHz, 298 K, CDCl3): delta = 7.37-7.33 (m, 2 H), 7.02-6.98(m, 3 H), 3.92 (d, 3J = 5.7 Hz, 2 H), 1.91-1.86 (m, 1 H), 1.61-1.31 (m,24 H), 1.02-0.99 (m, 6 H). 13C NMR (100 MHz, 298 K, CDCl3): delta = 159.4, 129.3, 120.3, 114.5, 70.7,38.0, 32.0, 31.9, 31.5, 31.4, 30.1, 29.8, 29.6, 29.4, 26.9, 26.9, 22.7, 14.1. MS (EI): m/z calcd for C22H38O+: 318.3; found: 318.3 [M+], 225.2 [M -OC6H5]+.

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 52997-43-0.

Reference:
Article; Bothe, Michael; Montero-Rama, Maria Pilar; Viterisi, Aurelien; Cambarau, Werther; Stenta, Caterina; Palomares, Emilio; Marsal, Lluis F.; Von Delius, Max; Synthesis; vol. 50; 4; (2018); p. 764 – 771;,
Bromide – Wikipedia,
bromide – Wiktionary

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

To a 1 L reaction flask was added toluene solvent (450 ml), 2,8-dibromodibenzofuran (11.74 g, 36 mmol),Intermediate I-21 (36.22 g, 90 mmol), Pd2 (dba) 3 (990 mg, 1.08 mmol),BINAP (1.65 g, 16.5 mmol) and sodium tert-butoxide (9.9 g, 100.8 mmol),Dissolved by stirring, and refluxed under nitrogen for 24 hours.After completion of the reaction, the reaction solution was washed with dichloromethane and distilled water and then evaporated.The organic layer was dried over anhydrous magnesium sulfate. After filtered, solvent was removed, and purified by column chromatography using cyclohexane: ethyl acetate = 10:1 as eluent.Finally, solid compound 21 (25.81 g, yield 74%) was obtained, and the solid purity was 99.6% by HPLC.

The synthetic route of 2,8-Dibromodibenzo[b,d]furan has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Changchun Hai Purunsi Technology Co., Ltd.; Zhao Qian; Liu Hui; Han Chunxue; (55 pag.)CN110407829; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

61921-39-9, A common compound: 61921-39-9, name is 4-Bromotetraphene, belongs to bromides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below.

Example 54 Synthesis of 4-(diphenylamino)benz[a]anthracene 190 mul (1 mmol) of chlorodi-tert-butylphosphine and then 112 mg (0.5 mmol) of palladium(II) acetate are added to a suspension of 15.4 g (50 mmol) of 4-bromobenz[a]anthracene, 10.2 g (60 mmol) of diphenylamine and 7.7 g (80 mmol) of sodium tert-butoxide in 500 ml of toluene, and the mixture is subsequently heated under reflux for 5 h. After the mixture has been cooled to 60 C., 500 ml of water are added, the organic phase is separated off, filtered through silica gel, evaporated virtually to dryness at 80 C. in vacuo, and 300 ml of ethanol are then added. After cooling, the solid is filtered off with suction. Recrystallisation five times from dioxane (about 8 ml/g); sublimation (p=5*10-5 mbar, T=280 C.). Yield: 12.7 g (32 mmol), 64.1%, purity 99.9% (HPLC), Tg=74.7 C.

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

Reference:
Patent; Stoessel, Philipp; Buesing, Arne; Heil, Holger; US2010/187505; (2010); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

A common heterocyclic compound, 344-03-6, name is 1,4-Dibromotetrafluorobenzene, molecular formula is C6Br2F4, 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. 344-03-6.

Synthesis of 3,3′,3″,3″‘-(3,6-dibromobenzene-1,2,4,5-tetrayl)tetrapyridine (1) To a stirred solution of 3-bromopyridine (1.0 g, 6.3 mmol) in anhydrous THF (30 mL) is dropwise added n-butyllithium (1.6M in hexane, 5.9 mL, 9.5 mmol) under nitrogen at -78¡ã C. After 1 h stirring, 1,4-dibromo-2,3,5,6-tetrafluorobenzene (0.43 g, 1.4 mmol) is added in a portion. Then, the reaction temperature is allowed to room temperature and stirs overnight. The reaction solution is quenched with water (200 mL), and the resulted mixture is extracted with chloroform. The combined organic layers are washed with brine, dried over anhydrous Na2SO4, filtered and concentrated. The mixture is purified on silica gel column chromatography using 5:1 (v/v) hexane/chloroform as eluent to give a white solid.

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

Reference:
Patent; Kyulux, Inc.; Aguilera-Iparraguirre, Jorge; Gomez-Bombarelli, Rafael; Hirzel, Timothy D.; Cheng, Shuo-Hsien; Suzuki, Yoshitake; Yang, Yu Seok; (108 pag.)US2019/58130; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary