Tag: M.W=300-400

Some common heterocyclic compound, 61203-48-3, name is 2-Iodo-4,5-dimethoxybenzoic acid, molecular formula is C9H9IO4, 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: 61203-48-3

Examples 2.a-6.a[152] The intermediate 4-amino-6,7-methylenedioxycinnoline o-iodobenzamide derivatives used in Examples 2-6 were prepared using the following general procedure. [153] A 2.0M solution of oxalyl chloride in CH2Cl2 (1.3 equiv.) was added to a solution of 2-iodo-4,5-dimethoxybenzoic acid (1.0 equiv.) in anhydrous CH2Cl2 (§ 60 mL per 10 mmol benzoic acid) and the solution stirred at reflux for 3 h. The mixture was allowed to cool and was then concentrated to dryness in vacuo. To the residues was added a solution of requisite 4-amino-6,7-dimethoxyquinoline (1.0 equiv), triethylamine (2 equiv.) in CH2Cl2 (§ 60 mL per 4 mmol aminoquinoline). The reaction mixture was then stirred at reflux under N2. The reaction mixture was cooled and washed with sat. NaHCO3 and extracted with 3% HCl. The aqueous layer was neutralized with 20% NaOH and extracted with CHCl3, dried (MgSO4) and evaporated. [154] Example 2.a. N-(6,7-Methylenedioxycinnolin-4-yl)-N-(N,N-diethylaminoethyl)- 2-iodo-4,5-dimethoxybenzamide: Prepared from N’-(6,7-Methylenedioxycinnolin-4- yl)-N,N-diethylethane-1,2-diamine (640 mg, 2.2 mmol); (87% yield); reaction time 16 h; IR (CHCl3) 1656; 1H NMR (CDCl3) 0.92 (t, 6H, J=7.0), 2.50 (q, 4H, J=7.0), 2.80 (t, 2H, J=6.8), 3.39 (s, 3H), 3.71 (s, 3H), 3.94 (m, 1H), 4.41 (m, 1H), 6.21 (d, 2H, J=1.4), 6.39 (s, 1H), 7.01 (s, 1H), 7.39 (s, 1H), 7.64 (s, 1H), 9.11 (s, 1H); 13C NMR (CDCl3) 11.6, 46.9, 47.8, 51.1, 55.7, 56.1, 82.9, 96.9, 102.9, 105.5, 110.9, 122.1, 122.9, 133.0, 136.5, 144.9, 148.3, 150.1, 150.9, 151.7, 152.3, 169.8; HRMS calcd for C24H27O5N41H: 579.1105; found: 579.1105.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 61203-48-3, its application will become more common.

Reference:
Patent; GENZYME CORPORATION; TEICHER, Beverly A.; SCHMID, Steven M.; WO2012/15875; (2012); A1;,
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Reference of 175278-11-2, 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. 175278-11-2, name is 1-Bromo-3,5-difluoro-2-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a cooled solution of l-bromo-3,5-difluoro-2-iodobenzene (3.00 g, 9.41 mmol) in THF (15 mL, 0.63 M) at -20 C was added a solution of iPrMgCl (2M in THF, 6.12 mL, 12.23 mmol) dropwise. The mixture was stirred for 10 min and then warmed to 0 C and stirred an additional 50 min. Copper iodide (0.448 g, 2.35 mmol) was added, and the reaction was stirred for 10 min. 3-bromo-2-methylprop-l-ene (1.04 mL, 10.4 mmol) was added, and the mixture was warmed to room temperature and stirred overnight. The reaction was quenched with sat. aq. NH4C1 (20 mL), diluted with EtOAc (20 mL) and extracted with EtOAc (3 x 10 mL). The combined organics were washed with brine (2 x 20 mL), dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo. The resulting residue was purified by silica gel column (100% Hex) to give the desired product l-bromo-3,5- difluoro-2-(2-methylallyl)benzene as a colorless and clear oil (1.60 g). Yield 69%.

The synthetic route of 1-Bromo-3,5-difluoro-2-iodobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MORPHIC THERAPEUTICS, INC.; HARRISON, Bryce, A.; DOWLING, James, E.; GERASYUTO, Aleksey I.; BURSAVICH, Matthew, G.; TROAST, Dawn, M.; LIPPA, Blaise, S.; ROGERS, Bruce, N.; ZHONG, Cheng; QIAO, Qi; LIN, Fu-Yang; SOSA, Brian; BORTOLATO, Angrea; SVENSSON, Mats, A.; HICKEY, Eugene; DAY, Tyler; KIM, Byungchan; (163 pag.)WO2020/47207; (2020); A1;,
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Some common heterocyclic compound, 628-77-3, name is 1,5-Diiodopentane, molecular formula is C5H10I2, 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. SDS of cas: 628-77-3

The tetra-TTF calix[4]pyrroles 2a-i (porphyrinogen derivatives of the present invention) were synthesized as shown in Schemes 3-1 1. Treating the monopyrroIo-TTF derivatives 1a- i with an excess of TFA and in the presence or absence of tetrabutylamonium fluoride (TBAF), tetrabutySarnonium chloride (TBACI), or tetrabutylamonium bromide (TBABr) in a mixture of CH2CI2 and Me2CO gave the tetra-TTF ca I ix[4] pyrroles 2a-i as yellow compounds in 13-55% yields. The tetra-TTF calix[4]pyrroles 2a-i were fully characterized by traditional techniques. The required monopyrrolo-TTF derivatives 1a-b were prepared according to the literature procedures (Hansen et a/ J Mater. Chem, 2004, 14, 179-184 and Jeppesen ef a/. J Org Chem. 2000, 65, 5794-5805), whereas the monopyrroio-TTF derivatives 1c- i were prepared as illustrated in Schemes 12-18.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 628-77-3, its application will become more common.

Reference:
Patent; SYDDANSK UNIVERSITET; WO2007/132430; (2007); A2;,
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Application of 628-77-3, A common heterocyclic compound, 628-77-3, name is 1,5-Diiodopentane, molecular formula is C5H10I2, 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 dry argon-flushed flask was charged with 2 (302 mg,1 mmol) and anhydrous THF (18 ml). The solution wascooled to 0 C and n-BuLi (1.18 ml, 2 mmol, 1.7 M solutionin THF) was added dropwise over 10 min and the reactionmixture was stirred for 1 h. In a second flask 1,5-diiodopentaneor 1,10-diiododecane (6 mmol) was dissolved in 3 mlof dry THF and added to the solution of lithiated speciesvia a cannula. The reaction mixture was allowed to reachroom temperature and was stirred for 3 h before quenchedwith a saturated solution of NH4Cl(30 ml). The aqueouslayer was extracted with hexane (3 × 25 ml). The combinedorganic layers were washed with brine (1 × 50 ml), water(1 × 50 ml), dried over MgSO4and filtered. Solvents wereevaporated under reduced pressure and the crude reactionmixture was purified by column chromatography on silicagel using hexane:EtOAc as the mobile phase with a gradientelution mixture (20:1, 10:1, 5:1).

The synthetic route of 628-77-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Luka?ek, Jan; ?ezankova, Marketa; Stibor, Ivan; ?ezanka, Michal; Journal of Inclusion Phenomena and Macrocyclic Chemistry; vol. 92; 3-4; (2018); p. 339 – 346;,
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Synthetic Route of 31827-94-8, 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. 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: The appropriate carbonyl compound (50 mmol) was dissolved in 50 mL of ethanol and magnetically stirred with an equimolar quantity of thiosemicarbazide for 24 h at room temperature with catalytic amounts of acetic acid. The desired thiosemicarbazone precipitated from reaction mixture, was filtered, crystallized from suitable solvent, and dried. Equimolar quantities of 4-iodo-acetophenone and bromine, both dissolved in chloroform, were stirred for 4 h at room temperature until the presence of HBr disappeared. The solution was evaporated under vacuum and the obtained pale yellow solid was washed with petroleum ether to give alpha-bromo-4-iodo-acetophenone in good yield (94%). Equimolar amounts of the prepared thiosemicarbazone (50 mmol) and alpha-bromo-4-iodo-acetophenone (50 mmol), both suspended in 50 mL of ethanol, were reacted at room temperature under magnetic stirring for 10 h. The precipitate was filtered and purified by chromatography to give compounds 1-25 in high yield.

The chemical industry reduces the impact on the environment during synthesis 2-Bromo-1-(4-iodophenyl)ethanone. I believe this compound will play a more active role in future production and life.

Reference:
Article; Secci, Daniela; Bizzarri, Bruna; Bolasco, Adriana; Carradori, Simone; D’Ascenzio, Melissa; Rivanera, Daniela; Mari, Emanuela; Polletta, Lucia; Zicari, Alessandra; European Journal of Medicinal Chemistry; vol. 53; (2012); p. 246 – 253;,
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Reference of 34270-90-1, These common heterocyclic compound, 34270-90-1, name is 1-Iodo-2-(2-iodoethoxy)ethane, 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.

Step 1 :NaH (60% in oil, 975 mg, 24.38 mmol) is washed with pentane (3x) and then suspended in dry THF (10 mL). A solution of 4,4-dimethyl cyclohexanone (1.02 g, 8.12 mmol, Combi-Blocks) in THF (5 mL) is added, followed by bis-2-iodoethyl ether (1.25 mL, 8.80 mmol). The reaction mixture is heated to 65C. When an exothermic reaction occurs, external heating is stopped and the reaction mixture is stirred for 1.5 h. The reaction mixture is heated at reflux for 30 min, and then is poured into water and extracted with ether. The aqueous phase is acidified to pH 6 with 1 M HCI and extracted with ether (2x). The filtrate is dried over anhydrous Na2S04, concentrated under reduced pressure and purified by Combiflash (90:10Hex EtOAc) to afford 6a1.

The synthetic route of 34270-90-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; BROCHU, Christian; GRAND-MAITRE, Chantal; FADER, Lee; KUHN, Cyrille; BERTRAND-LAPERLE, Megan; PESANT, Marc; WO2013/26163; (2013); A1;,
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Reference of 19821-80-8, A common heterocyclic compound, 19821-80-8, name is 1,3-Dibromo-2-iodobenzene, molecular formula is C6H3Br2I, 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.

2,6-dibromoiodobenzene (1.0 g, 2.8 mmol), 1-naphthaleneboronic acid (0.48 g, 2.8 mmol),Tetrakis(triphenylphosphine)palladium (0.33 g, 0.28 mmol), lithium hydroxidemonohydrate (0.46 g, 11 mmol) were charged into a flask, and purged 3 times with nitrogen,the degassed acetonitrile (100 mL) and degassed water (10 mL) were added, and stirred at 70C for 14 hunder nitrogen atmosphere. The reaction mixture was cooled to room temperature and diluted with EtOAcand H2O, then separated and the organic layer was dried over Na2SO4 and concentrated under reducedpressure. The residue was purified by column chromatography on silica gel to give the desired product(0.69 g, 69%). 1H NMR (500 MHz, CDCl3): 7.95-7.91(m, 2H), 7.71 (d, J = 8.0 Hz, 2H), 7.58 (t, J = 8.0Hz, 1H), 7.51 (t, J = 8.0 Hz, 1H), 7.43 (t, J = 8.0 Hz, 1H), 7.34-7.30 (m, 2H), 7.18 (t, J = 8.0 Hz, 2H);13C NMR (125 MHz, CDCl3) 141.5, 138.9, 133.5, 131.9, 130.9, 130.2, 128.6, 128.5, 127.0, 126.5, 126.1,125.5, 125.4, 124.9; HRMS (EI-TOF): Calcd for C16H10Br2, 359.9149; found 359.9152.

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; Zhou, Haifeng; Uozumi, Yasuhiro; Synlett; vol. 24; 19; (2013); p. 2550 – 2554;,
Iodide – Wikipedia,
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Reference of 450412-28-9, 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. 450412-28-9, name is 1-Bromo-3-chloro-2-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

1-bromo-3-chloro-2-iodobenzene 200.00 g (1.0 eq),2-aminophenol 68.77 g (1.0 eq), K3PO4 267.55 g (2.0 eq),1.61 g (0.005 eq) of Pd (t-Bu3P) 2 was dissolved in 1.5 L of toluene, refluxed and stirred.The solution was concentrated under reduced pressure for 3 hours.After that, it was completely dissolved in CHCl3, washed with water and decompressed again to remove about 50% of the solvent. Ethyl acetate was added in the refluxing state, and the crystals were dropped, cooled, and filtered. This was subjected to column chromatography to obtain 137.35 g (yield 73%) of a compound represented by the formula 7-a.

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, 1-Bromo-3-chloro-2-iodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; LG Chem, Ltd.; Kim Min-jun; Park Tae-yun; Cho Seong-mi; Lee Jeong-ha; (88 pag.)KR2017/113319; (2017); A;,
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Synthetic Route of 4897-68-1,Some common heterocyclic compound, 4897-68-1, name is 1-Bromo-2-iodo-4-methoxybenzene, molecular formula is C7H6BrIO, 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.

The 135mg (1mmol) benzothiazole, 376mg (1.2mmol) 1- bromo-2-iodo-4-methoxybenzene, 2.5mg (0.01mmol) CuSO4·5H2O, 19.4mg (0.1mmol) ligand L4,240mg (6mmol) NaOH, 2gPEG-600, was added 10mL reaction tube, sealed, under the reaction condition of 80 14h.After the reaction was stopped, extraction with ethyl acetate, washed with water, brine, dried over anhydrous sodium sulfate, filtered, and the filtrate was evaporated under reduced pressure, purified by silica gel column chromatography separation and purification, to give 3-methoxy-phenothiazine 172mg, yield 75%.

The synthetic route of 4897-68-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sun Yat-sen University; Wan, Yiqian; Huang, Manna; Huang, Dongting; Zhu, Xinhai; (11 pag.)CN104529938; (2016); B;,
Iodide – Wikipedia,
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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. 755027-18-0, name is 1-Bromo-4-iodo-2-methoxybenzene, A new synthetic method of this compound is introduced below., Safety of 1-Bromo-4-iodo-2-methoxybenzene

One-neck round bottom flask (One neck r.bf)on1-Bromo-4-iodo-2-methoxybenzene(50 g, 159.7 mmol),Triphenylene-2-ylboronic acid (500 mL / 100 mL), potassium carbonate (44.1 g, 319 mmol), 1,4-dioxane / water (43 mL), tetrakis (triphenylphosphine) palladium (0) (9.2 g, 7.89 mmol) The mixture was refluxed at 110 & lt; 0 & gt; C.Extraction with dichloromethane & lt; RTI ID = 0.0 & gt; MgS04 & lt; / RTI & gt;Filtered through silica gel and concentrated to give the compound 4-5-5. (48 g, 72%).

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:
Patent; L Ti Material Co., Ltd.; Park Geon-yu; Noh Yeong-seok; Yang Seung-gyu; Cha Ju-hyeon; Kim Dong-jun; Choi Dae-hyeok; Lee Ju-dong; (100 pag.)KR2019/30963; (2019); A;,
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