Iodides-buliding-blocks

Reference of 33348-34-4, A common heterocyclic compound, 33348-34-4, name is 4-Amino-3-iodobenzonitrile, molecular formula is C7H5IN2, 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.

Description for D20; delta-Cyano-IH-indole^-carboxylic acid (D20); A suspension of 4-amino-3-iodobenzonitrile (2.44 g), 2-oxopropanoic acid (2.64 g), DABCO (3.36 g), and Pd(OAc)2 in DMF (30 ml.) was heated to 105 0C and stirred at that temperature for 1 hour. The solvent was evaporated. EtOAc (200 ml.) was added and the resulting solution was washed with water (100 ml.) and aqueous NaOH solution (20 ml_). The combined aqueous solution was extracted with EtOAc (3 x 150 ml_). The organic fractions were combined. The combined solution was dried over anhydrous magnesium sulfate. The dried solution was concentrated. The residue was triturated to afford 5-cyano-1 /-/-indole-2-carboxylic acid (D20) (1.1 g) as a brown solid.

The synthetic route of 33348-34-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; WO2009/153307; (2009); A1;,
Iodide – Wikipedia,
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Electric Literature of 628-77-3, These common heterocyclic compound, 628-77-3, name is 1,5-Diiodopentane, 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: To a dry, nitrogen purged flask was charged with compound 2-1 (26.5 g, 0.1 mol,1.0 eq), compound 1-3 (17.8 g, 0.1 mol, 1.0 eq), potassium t-butoxide (13.4 g, 0.12 mol, 1.2 eq),anhydrous THF (450 ml).The mixture was stirred at 50 & lt; 0 & gt; C for 16 hrs.Add excess ammonium acetate, acetic acid.The mixture was refluxed for 16 hrs.After cooling to room temperature, the reaction solution was spin dried,and 600 ml of deionized water and 600 ml of ethyl acetatewere added to the residueand then stirred at 30 C for 30 mins.The organic phase was separated from the aqueous phasewhile the organic phase was washed three times with water (600 ml) and washed with saturated brine three times (600 ml).The organic phase wasdriedoveranhydrous sodium sulfate and filtered to dryness.The resulting crude product was purified by column chromatography usingethyl acetate / petroleum ether (1: 5 by volume) as a mobile phaseand vacuum dried at 50 C to give the first intermediate of the compound.The resulting intermediate intermediate 1-3 (37.9 g, 0.1 mol, 1.0 eq),compound 2-2 (71.3 g, 0.22 mol, 2.2 eq), potassium tert- 24.6 g, 0.22 mol, 2.2 eq), anhydrousTHF (250 mL).The mixture was stirred under nitrogen at 50 C for 16 hrs.After cooling to room temperature, thereaction solution was spin dried, and 600 ml of deionized water and 600 ml of ethyl acetate were added to the residue and thenstirredat 30 Cfor 30 mins.The organic phase was separated from the aqueous phase while the organic phase was washed three times with water (600 ml)and washedwith saturatedbrine three times (600 ml).The organic phase was dried over anhydrous sodium sulfate and filtered to dryness.Residue with ethylacetate / petroleum ether (volume ratio of 1: 6) as mobile phase The resultant crude product was purified by column chromatography at 50 deg.] Cto give compound 2-3 (35.4g after drying in vacuo to yield 79.02 %).

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

Reference:
Patent; Shanghai Hehui Optoelectric Co., Ltd.; Yan Liangliang; Gong Zhihao; Li Weimeng; (14 pag.)CN106939024; (2017); A;,
Iodide – Wikipedia,
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Some common heterocyclic compound, 58313-23-8, name is Ethyl-3-iodobenzoate, molecular formula is C9H9IO2, 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. Safety of Ethyl-3-iodobenzoate

Ethyl 3-iodobenzoate (0.92 g, 3.34 mmol, 1 eq.), phenylboronic acid (0.87 g, 5.02 mmol, 1.5 eq.), palladium(II)acetate (37 mg, 0.167 mmol, 0.05 eq.) and sodium carbonate (706 mg, 6.66 mmol, 2 eq.) were dissolved in DMF (20 mL) at room temperature under nitrogen. The reaction was then heated at 80 C. for 1.5 hours. Worked up by adding ethyl acetate and rinsing 4 times with water. The organic layer was dried over sodium sulfate and stripped to give a dark oil. Purified over silica gel in 9:1 to 1:1 hexanes/ethyl acetate to obtain 3′-Amino-[1,1′-biphenyl]-3-carboxylic acid, ethyl ester (420 mg) as an oil. Yield=55%. LCMS detects (M+H)+=242.41.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 58313-23-8, its application will become more common.

Reference:
Patent; Carter, Percy H.; Cherney, Robert J.; Batt, Douglas G.; Duncia, John V.; Gardner, Daniel S.; Ko, Soo S.; Srivastava, Anurag S.; Yang, Michael G.; US2005/54627; (2005); A1;,
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Application of 69113-59-3, These common heterocyclic compound, 69113-59-3, name is 3-Iodobenzonitrile, 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: Step 1: 3-{[1-(6,7-dimethoxyquinazolin-4-yl)piperidin-4-yl]methyl}-3,4-dihydroquinazolin-2(1H)-one (50 mg, 0.12 mmol) obtained by the method described in Chemical & Pharmaceutical Bulletin 1990, 38(6), 1591, copper(I) iodide (22 mg, 0.12 mmol), trans-1,2-cyclohexanediamine (13 mg, 0.12 mmol), 3-iodobenzonitrile (53 mg, 0.23 mmol) and tripotassium phosphate (49 mg, 0.23 mmol) were stirred in 1,4-dioxane (1.0 mL) at 100 C. for 5 hours. To the reaction mixture, a saturated aqueous sodium bicarbonate solution was added, and the resulting mixture was extracted with ethyl acetate. The organic layer was treated with diatomaceous earth and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (a chloroform/methanol mixed solvent), whereby the title Compound 6 (51 mg, yield: 82%) was obtained. ESI-MS m/z: 535 (M+H)+, 1H-NMR (300 MHz, CDCl3, delta): 8.66 (s, 1H), 7.73-7.59 (m, 4H), 7.24 (s, 1H), 7.16-7.00 (m, 4H), 6.17 (d, J=8.4 Hz, 1H), 4.62 (s, 2H), 4.24-4.14 (br m, 2H), 4.02 (s, 3H), 3.98 (s, 3H), 3.47 (d, J=7.3 Hz, 2H), 3.10-3.06 (br m, 2H), 2.18-2.10 (m, 1H), 1.93-1.90 (m, 2H), 1.62-1.54 (m, 2H)

The synthetic route of 69113-59-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; KYOWA HAKKO KIRIN CO., LTD.; ISHIDA, Hiroshi; MOTOSAWA, Keiichi; MIURA, Yusuke; NAKAI, Ryuichiro; OKADA, Ryoko; TAKAHASHI, Yuichi; (45 pag.)US2016/168125; (2016); A1;,
Iodide – Wikipedia,
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Electric Literature of 17024-12-3, The chemical industry reduces the impact on the environment during synthesis 17024-12-3, name is 9-Iodophenanthrene, I believe this compound will play a more active role in future production and life.

10261] Into an 80-mE flask were put 3.27 g (17 mmol) of3-chlorobenzamidine hydrochloride, 5.2 g (17 mmol) of 9-io- dophenanthren, 0.31 g (1.6 mmol) of copper iodide, 16 g (49 mmol) of cesium carbonate, 0.29 g (3.3 mmol) of N,N-dimethylethylenediamine, and 80 mE of dimethylformamide (DMF), and the air in the flask was replaced with nitrogen. The mixture in the flask was stirred at 1000 C. for 21 hours. Then, 0.31 g (1.6 mmol) of copper iodide and 0.29 g (3.3 mmol) of N,N-dimethylethylenediamine were added, and the mixture was stirred at 110 C. for 8.5 hours. The resulting solution was subjected to suction filtration, and the obtained solid was washed with toluene. The obtained filtrate was washed with water, and the organic layer was washed with saturated saline. Magnesium sulfate was added to the organic layer for drying, and the resulting mixture was subjected to gravity filtration to give a filtrate. The filtrate was condensed to obtain an objective substance (a brown oily substance, at a yield of 50%). The synthesis scheme of Step 1 is shown in (a-i).

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

Reference:
Patent; Semiconductor Energy Laboratory Co., Ltd.; HARA, Tomoka; INOUE, Hideko; TAKAHASHI, Tatsuyoshi; HAMADA, Takao; SEO, Satoshi; (60 pag.)US2016/190479; (2016); A1;,
Iodide – Wikipedia,
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Some common heterocyclic compound, 755027-18-0, name is 1-Bromo-4-iodo-2-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. Recommanded Product: 1-Bromo-4-iodo-2-methoxybenzene

Step 2: ethyl 2-(4-bromo-3-methoxyphenyl)cyclohex-1-ene-1-carboxylate To a solution of the product from Step 1, ethyl 2-{[(trifluoromethyl)sulfonyl]oxy}cyclohex-1-ene-1-carboxylate (6.65 g, 22.0 mmol) in dioxane (125 mL) was added potassium carbonate (4.56 g, 33.0 mmol), PPh3 (0.346 g, 1.32 mmol), bis(pinacolato)diboron (6.15 g, 24.20 mmol), and PdCl2(PPh3)2 (0.463 g, 0.66 mmol). The mixture was then heated to 80 C. overnight. This solution was then cooled to r.t. and added to a mixture of 1-bromo-4-iodo-2-methoxybenzene (6.86 g, 21.92 mmol), PdCl2(dppf) (0.481 g, 0.657 mmol), potassium carbonate (9.09 g, 65.7 mmol). This mixture was then heated to 80 C. overnight. The mixture was then cooled to r.t., diluted with EtOAc (300 mL) and washed with brine and aqueous KHSO4. The organic layer was then dried over Na2SO4 and the solvent was removed in vacuo. The crude material was then purified on silica (100% DCM) to give impure product which was repurified on silica (gradient elution, 5-20% EtOAc/hexanes) to give the title compound.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 755027-18-0, its application will become more common.

Reference:
Patent; Harper, Steven; Summa, Vincenzo; Liverton, Nigel J.; McCauley, John A.; Butcher, John W.; Di Filippo, Marcello; Di Francesco, Maria Emilia; Ferrara, Marco; Romano, Joseph J.; Rudd, Michael T.; US2010/183551; (2010); A1;,
Iodide – Wikipedia,
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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 260355-20-2 as follows. SDS of cas: 260355-20-2

General procedure: reaction vial (8 ml) was charged with benzoazine (0.10 mmol, 1.0 equiv.), template-MeCN (0.10 mmol, 1.0 equiv.) and 0.2 ml dichloromethane. The mixture was stirred for 5 min at room temperature, and then concentrated in vacuo. Pd(OAc)2 (2.2 mg,10 mumol, 10 mol%), Ac-Gly-OH (2.3 mg, 20 mumol, 20 mol%), aryl iodide (0.3 mmol,3 equiv.), AgOAc (50 mg, 0.30 mmol, 3.0 equiv.), Ag2CO3 (27.6 mg, 0.1 mmol,1.0 equiv.), NBE-CO2Me (22.8 mg, 0.15 mmol, 1.5 equiv.) and HFIP (1.5 ml) were added. The reaction vial was sealed and allowed to stir at 80 C for 18 h. The reaction mixture was cooled to room temperature. Then a solution of DMAP (36.7 mg, 0.3 mmol, 3 equiv.) in toluene (1.5 ml) was added. The mixture was stirred at 80 C for 15 min. The reaction mixture was cooled to room temperatureand diluted with EtOAc. The mixture was filtered through a short pad of celite and eluted with EtOAc (2 ¡Á 2 ml). The filtrate was evaporated under reduced pressure. (If the product release was not complete, a solution of DMAP (18.4 mg,0.15 mmol, 1.5 equiv.) in toluene (1.5 ml) was added; the solution was then stirredat 80 C for 15 min and then concentrated.) Purification by preparative thin-layer chromatography afforded the title compound

According to the analysis of related databases, 260355-20-2, the application of this compound in the production field has become more and more popular.

Reference:
Article; Bay, Katherine L.; Chen, Xiangyang; Houk, Kendall N.; Lu, Yi; Shi, Hang; Tanaka, Keita; Verma, Pritha; Weng, Jiang; Yu, Jin-Quan; Nature Chemistry; (2020);,
Iodide – Wikipedia,
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Related Products of 34270-90-1, 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. 34270-90-1, name is 1-Iodo-2-(2-iodoethoxy)ethane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Disulfide 18 (82 mg, 0.105 mmol) was treated with NaBH4 (15 mg, 0.39 mmol) in dry DMF (1 mL) for 10 min before a solution of 35 (34 mg, 0.104 mmol) in dry DMF (1 mL) was added. The reaction mixture was stirred at room temperature for 1 h and then diluted with mildly acidic H2O. The aqueous phase was extracted four times with CH2Cl2 before the combined organic phases were concentrated in vacuo. The residue was dissolved in EtOAc and washed five times with H2O. The organic phase was dried over MgSO4, filtered and concentrated under reduced pressure. The crude product was purified by column chromatography (EtOAc/CH2Cl2 1:2) to afford 6 as white solid (24 mg, 27%): Rf: 0.24 (EtOAc/CH2Cl2 1:2); 1H NMR (400 MHz, CDCl3): deltaH 5.87 (s, 1H, H22), 4.98 (dd, 1H, J17,21a 1.6 Hz, Jgem 18.0 Hz, H21a), 4.80 (dd, 1H, J17,21b 1.6 Hz, Jgem 18.0 Hz, H21b), 3.60 (t, 2H, J24,25 7.0 Hz, H25), 3.25 (br s, 1H, H3), 2.77 (m, 1H, H17), 2.67 (t, 2H, J24,25 7.0 Hz, H24), 2.12 (m, 2H), 1.90-1.17 (m, 19H), 0.94 (s, 3H, CH3), 0.86 (s, 3H, CH3); 13C NMR (100 MHz, CDCl3): deltaC 174.7 (C20, C23), 117.8 (C22), 85.7 (C14), 73.6 (C21), 70.9 (C25), 51.0, 49.7 (C13, C17), 44.0, 42.0, 40.1, 37.2, 36.1, 35.7, 33.3, 31.8, 31.3, 30.9, 27.0, 26.9, 26.2, 23.8, 21.7, 21.2, 15.9; HRMS (ES): Calcd for C50H74O7S2Na 873.4773, found 873.4814.

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-Iodo-2-(2-iodoethoxy)ethane, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Jensen, Marie; Schmidt, Steffen; Fedosova, Natalya U.; Mollenhauer, Jan; Jensen, Henrik H.; Bioorganic and Medicinal Chemistry; vol. 19; 7; (2011); p. 2407 – 2417;,
Iodide – Wikipedia,
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Application of 39998-81-7, These common heterocyclic compound, 39998-81-7, name is 2-Fluoro-4-iodo-1-methylbenzene, 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-Fluoro-4-iodobenzoic acid, m.p. 213-215 C. (dec) is similarly prepared from 2-fluoro-4-iodotoluene.

Statistics shows that 2-Fluoro-4-iodo-1-methylbenzene is playing an increasingly important role. we look forward to future research findings about 39998-81-7.

Reference:
Patent; The Trustees of Princeton University; US4889859; (1989); A;,
Iodide – Wikipedia,
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Electric Literature of 13421-00-6,Some common heterocyclic compound, 13421-00-6, name is 5-Chloro-2-iodobenzoic acid, molecular formula is C7H4ClIO2, 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.

Borane-dimethylsulfide complex (3.7 mL, 38.9 mmol) was added slowly to a cold (0C) solution of 5-chloro-2-iodo-benzoic acid (10 g, 35.4 mmol) in THF (20 mL). The reaction mixture was allowed to warm to rt, stirred for 8 h, quenched by addition of a saturated aqueous solution of ammonium chloride, and extracted with EtOAc. The organic layer was dried (Na2S04), filtered, and concentrated to provide 9.5 g of the title compound. tR: 4.72 min (HPLC 2); Rf= 0.66 (hexane/EtOAc, 7:3).

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

Reference:
Patent; NOVARTIS AG; FURET, Pascal; GUAGNANO, Vito; HOLZER, Philipp; MAH, Robert; MASUYA, Keiichi; SCHLAPBACH, Achim; STUTZ, Stefan; VAUPEL, Andrea; WO2013/80141; (2013); A1;,
Iodide – Wikipedia,
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