Tag: M.W=200-300

Reference of 51554-93-9, These common heterocyclic compound, 51554-93-9, name is 1-Bromo-4-octylbenzene, 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.

Phenothiazine (2.37 g, 11.9 mmol), 1-bromo-4-n-octyl-benzene (4.17 g, 15.4 mmol) and sodium tert-butoxide (2.3 g, 23.8 mmol) are dissolved sufficiently in 50 mL of toluene.Tri tert-butylphosphine(0.144 g, 0.7 mmol)And Pd2 (dba) 3 (0.54 g, 0.59 mmol)After sufficiently dissolving at room temperature under a nitrogen atmosphere,And the mixture is stirred at 120 C under reflux.When the reaction is complete, work-up is carried out with a 1: 1 mixture of water and chloroform.After separating the organic layer after the work-up process using the extraction method,The solvent is removed under reduced pressure.After the solvent was removed, the product was recrystallized several times with methanol to obtain a pale yellow solid product (3.5 g, 76%) was obtained.

The synthetic route of 51554-93-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Daegu Gyeongbuk Institute of Science and Technology Foundation; Jo, Hyo Jung; Kang, Jin Kyu; Nam, Jung Eun; Kim, Dae Hwan; (11 pag.)KR101526327; (2015); B1;,
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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. 13633-25-5, name is 1-Bromo-4-phenylbutane, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 1-Bromo-4-phenylbutane

To a stirred solution of tert-Butylprop-2-yn-1-ylcarbamate (300 mg, 1.93 mmol, 1 eq.) in dry DMF (1.93 mL) under nitrogen at 0C, was added NaH (93 mg, 60% in oil, 2.32 mmol, 1.2 eq.) in small portions. After stirring for 15min, (4-bromobutyl)benzene (410 muL, 2.34 mmol, 1.2 eq.) was added dropwise followed by KI(32 mg, 0.19 mmol, 0.1 eq.) and the reaction was warmed up to room temperature for 15 h.After completion of the reaction, water and brine were added and the aqueous layer wasextracted with Et2O (three times). Then, the combined organic layers were dried over MgSO4,filtered and concentrated under vacuum. The crude residue was purified by flash columnchromatography on silica gel (cyclohexane/DCM: 50/50) to afford 1h (446 mg, 1.54 mmol, 80%)as a colorless oil. 1H NMR (300 MHz, CDCl3): delta 7.31-7.24 (m, 2H), 7.21-7.14 (m, 3H), 4.01 (br. s,2H), 3.33 (t, J = 6.6 Hz, 2H), 2.64 (t, J = 7.1 Hz, 2H), 2.16 (t, J = 2.4 Hz, 1H), 1.67-1.56 (m, 4H),1.45 (s, 9H); 13C NMR (100 MHz, CDCl3): delta 155.2 (br. s), 142.4 (br. s), 128.5 (2C), 128.4 (2C),125.8, 80.2, 80.0 (br. s), 71.4 (br. s), 46.4, 36.4 and 36.0 (br. S, rot.), 35.6, 28.6 (br. s), 28.5 (3C),27.6 (br. s).

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 13633-25-5.

Reference:
Article; Guissart, Celine; Dolbois, Aymeric; Tresse, Cedric; Saint-Auret, Sarah; Evano, Gwilherm; Blanchard, Nicolas; Synlett; vol. 27; 18; (2016); p. 2575 – 2580;,
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Synthetic Route of 138526-69-9, A common heterocyclic compound, 138526-69-9, name is 1-Bromo-3,4,5-trifluorobenzene, molecular formula is C6H2BrF3, 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: A mixture of the styrene (3 mmol), the halogenated benzene (3 mmol), triethanolamine (3 mmol) and Pd (II) acetate (0.03 g) was stirred under argon at 100 C for 24 h. The reaction was cooled to 25 C, quenched by the addition of dil. aq. hydrochloric acid (2 N, 10 ml), and extracted with ether (3 × 100 ml). The organic phases were dried (Na2SO4), the solvents evaporated, and the crude product was subjected to chromatography (silica gel, hexane/ethyl acetate mixtures).

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; Csuk, Rene; Albert, Sabrina; Siewert, Bianka; Schwarz, Stefan; European Journal of Medicinal Chemistry; vol. 54; (2012); p. 669 – 678;,
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The chemical industry reduces the impact on the environment during synthesis 699-03-6, name is 1-(4-Bromophenyl)-N-methylmethanamine, I believe this compound will play a more active role in future production and life. 699-03-6

The prepared Formula-G was then dissolved in dichloromethane (1.8 L). Triethylamine (1.6 moles, 223.2 mL) was added at 5 C. A solution of methyl chloroformate (1.3 moles, 100.4 mL in dichloromethane (0.2 L) was slowly added, maintaining the temperature of the mixture between about 10 C and 14 C. The reaction solution was stirred at room temperature for 12 hours. Water was added to the reaction mass and the organic phase was separated and concentrated to afford a compound of Formula-E (wherein L=Br, P=methyl carbamate).

The chemical industry reduces the impact on the environment during synthesis 699-03-6. I believe this compound will play a more active role in future production and life.

Reference:
Patent; MYLAN LABORATORIES LTD; JAYACHANDRA, Sureshbabu; SETHI, Madhuresh; KAUSHIK, Vipin Kumar; RAVI, Vijaya, Krishna; TELAGAMSETTY, Bhaskar Kumar; (44 pag.)WO2019/130229; (2019); A1;,
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Some common heterocyclic compound, 185122-74-1, name is 5-Bromo-2,3-dihydro-1H-inden-1-amine, molecular formula is C9H10BrN, 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. Application In Synthesis of 5-Bromo-2,3-dihydro-1H-inden-1-amine

To a suspension of 5-bromo-2,3 -dihydro- lH-inden-1 -amine (2.2 g, 10.4 mmol) and NaHC03 (2.6 g, 31.2 mmol) in MeCN (100 mL) was added Boc20 (3.4 mL, 15.6 mmol) at 0 C. The reaction was stirred at rt overnight, then concentrated in vacuo. The residue was dissolved in EtOAc (100 mL). The resulted solution was washed with H20 (50 mL x 2), dried over anhydrous a2S04, filtered and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (v/v) =20/1) to give the title compound as a white solid (3.3 g, 100%). MS (ESI, pos. ion) m/z: 257 [M + H – 56]+; NMR (400 MHz, i/6-DMSO) delta (ppm): 1.48 (s, 9H), 1.72-1.85 (m, 1H), 2.49-2.62 (m, 1H), 2.77-2.88 (m, 1H), 2.89-2.98 (m, 1H), 4.67-4.77 (br, 1H), 5.07-5.17 (m, 1H), 7.18 (d, J= 8.0 Hz, 1H), 7.32 (d, J= 8.0 Hz, 1H), 7.36 (s, 1H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 185122-74-1, its application will become more common.

Reference:
Patent; CALITOR SCIENCES, LLC; SUNSHINE LAKE PHARMA CO., LTD; XI, Ning; WANG, Ruyong; WANG, Liang; WO2014/89324; (2014); A1;,
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Related Products of 608-30-0,Some common heterocyclic compound, 608-30-0, name is 2,6-Dibromoaniline, molecular formula is C6H5Br2N, 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 1 Synthesis of 2,6-dibromobenzenesulfonyl chloride A solution of 2,6-dibromoaniline (10 g, 39.8 mmol) in trifluoroacetic acid (60 mL) and conc. HCl (12 mL) was cooled to 0 C. in an ice bath and treated dropwise with a solution of sodium nitrate (3.4 g, 39.8 mmol) in water (3 mL) over a period of 60 min. To the resulting mixture was added a suspension of copper(I) chloride (2.6 g) and copper(II) chloride (2.6 g) in sulfurous acid (70 mL) and acetic acid (70 mL) over a period of 90 min. After the addition was complete the resulting mixture was stirred at ambient temperature for 45 min. The resulting white precipitate was collected by filtration and dried under the reduced pressure to afford 2,6-dibromobenzenesulfonyl chloride as the white powder (5.2 g, 39%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,6-Dibromoaniline, its application will become more common.

Reference:
Patent; Wexler, Ruth R.; Jacobson, Irina C.; US6399644; (2002); B1;,
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Reference of 4263-52-9, 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. 4263-52-9, name is Sodium 2-bromoethanesulphonate, This compound has unique chemical properties. The synthetic route is as follows.

Synthesis of intermediate II (1-delta-sulphoethyl,-2,3,3-trimethyl-5-sulphonamido indolenininium inner salt); [Show Image] 150 g of 2-bromoethanesulfonic acid sodium salt, Fluka, 1,5 1 of ethanol are mixed together, the mixture is then cooled to 5C and 29,2 g of hydrochloric acid gas are bubbled through the mixture. After that, the mixture is brought back to RT and left under stirring for 4 hours. After filtration of sodium chloride, the mixture is concentrated to dryness under vacuum. 1,6 g of 2-bromoethanesulfonic acid, obtained with the method reported above, 1,3 g of intermediate I, 0,7 g of triethylamine and 5 ml of butirronitrile are mixed together and heated to reflux for 20 hours. The mixture is then cooled to rrom temperature and 15 ml of acetone are added. The solid product is vacuum filtered and washed with methanol and acetone. The reaction yield is 50%.

The chemical industry reduces the impact on the environment during synthesis Sodium 2-bromoethanesulphonate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Ferrania Technologies S.p.A.; EP1810998; (2007); A2;,
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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. 344-04-7, name is 1-Bromo-2,3,4,5,6-pentafluorobenzene, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 344-04-7

C5F5Br (12.35 gm, 0.05 mol) dissolved in dry ether, was added drop wise to Mg (1.2 gm, 0.05 mol) turnings at 0C. The resulting Grignard solution was cooled to -100C and (3.78 gm, 0.0165 mol) SbCl3 dissolved in dry ether slowly added with constant stirring. This mixture was stirred30 for an additional hour at room temperature and subsequently refluxed for one hour more. The mixture was then cooled to 0C and treated with ice water containing NH4Cl and subsequently followed by the addition of 4 N HCl (1 ml) and stirred to make the solution acidic. The ether layer was separated and dried over Na2SO4 and evaporated to give (C6Fs)3Sb. Yield 3.11 gm, 30 %, m.p. 74C (found C; 34.5: Sb; 19.32) (calculated for Ci8Fi5Sb: C; 34.7: Sb; 19.54) The brownish layer was extracted with CHCl3 and after working up it in usual manner give another crop of (C6F5)3Sb. Yield 3.63 gm, 35 %, m.p. 74C (found C; 34.49:Sb ; 19.34) ( calculated for Ci8Fi5Sb: C; 34.7: Sb; 19.54)

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 344-04-7.

Reference:
Patent; COUNCIL OF SCIENTIFIC AND INDUSTRIAL RESEARCH; CHANDRASHEKAR, Krishnappa; BEHL, Hari, Mohan; KUMAR, Vishal; SIDHU, Om, Prakash; PUSHPANGADAN, Palpu; RAO, Chandana, Venkateswara; SHUKLA, Sanjeev, Kumar; RANJAN, Ashok; SAXENA, Arvind, Kumar; KANT, Ravi; SINGHAL, Kiran; RAJ, Prem; WO2006/67800; (2006); A1;,
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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. 21524-34-5, name is 2-Bromo-1,3,5-triisopropylbenzene, A new synthetic method of this compound is introduced below., Application In Synthesis of 2-Bromo-1,3,5-triisopropylbenzene

General procedure: The Suzuki reaction was performed in a 50 mL round-bottomed flask, aryl halide (0.5 mmol), arylboronic acid (0.65 mmol), K2CO3 (1 mmol), Complex 1 (0.2-1 mol%) and water (4 mL) were charged and stirred for the required time at room temperature for aryl bromides or at 100 C for aryl chlorides. After completion, the mixture was cooled down to room temperature, diluted with water (10 mL) and extracted with diethyl ether (3 × 15 mL). The organic layer was washed with brine (3 × 15 mL), dried over anhydrous Na2SO4. The crude products were chromatographed on silica gel (ethyl acetate/hexane).

The synthetic route of 21524-34-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Shahnaz, Nasifa; Puzari, Amlan; Paul, Bidisha; Das, Pankaj; Catalysis Communications; vol. 86; (2016); p. 55 – 58;,
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Electric Literature of 445303-69-5, 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 445303-69-5 as follows.

2-(3-Difluoromethyl-4-fluoro-phenyl)-4,4,5,5-tetramethyl-[1,3,2]dioxaborolane The title compound was obtained according to example 342 as a colorless oil (54% yield) using 4-bromo-2-difluoromethyl-1-fluoro-benzene and bis(pinacolato)diboron as the starting materials. MS: m/e=272 (M+).

According to the analysis of related databases, 445303-69-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Alanine, Alexander; Buettelmann, Bernd; Heitz Neidhart, Marie-Paule; Jaeschke, Georg; Pinard, Emmanuel; Wyler, Rene; US2002/151715; (2002); A1;,
Bromide – Wikipedia,
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