Iodides-buliding-blocks

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 101335-11-9 as follows. Formula: C6H3ClFI

Step 1. Ethyl 2-(4-(2-chloro-4-fluorophenyl)-4-hydroxycyclohexyl)acetate. A solution of n-butyllithium in hexanes (1.6 M, 81.4 mL, 130 mmol) was added dropwise to a solution of 2- chloro-4-fluoro-l-iodobenzene (16.6 mL, 130 mmol) in tetrahydrofuran (197 mL) at -78C. The reaction mixture was allowed to stir at -78C for 1 h before the addition of ethyl 2-(4- oxocyclohexyl)acetate (19.2 mL, 109 mmol) in one portion. The reaction was allowed to warm to room temperature and stirred at room temperature for 1 h. The reaction was quenched with a saturated solution of ammonium chloride (500 mL) and extracted with EtOAc (3 x 150 mL), combined organics dried (Na2S04) and concentrated under reduced pressure. The residue was purified by flash chromatography on silica, eluting with 0-40% EtOAc in hexanes to yield the product as a colorless oil (26.7 g, 78%). 1H NMR (400 MHz, CDCb) d 7.65 (dd, / = 8.86, 6.30 Hz, 1H), 7.21 – 7.09 (m, 1H), 7.03 – 6.94 (m, 1H), 4.27 – 4.07 (m, 5H), 2.62 – 2.47 (m, 2H), 2.46 – 2.18 (m, 10H), 2.15 – 1.82 (m, 6H), 1.78 – 1.34 (m, 7H), 1.34 – 1.22 (m, 7H). [M-H2O+H] = 283.1.

According to the analysis of related databases, 101335-11-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; DART NEUROSCIENCE, LLC; BASINGER, THOMPSON, Jillian; BOOKSER, Brett; BURLEY, Scott; GARCIA-REYNAGA, Pablo; HUDSON, Andrew; PETERS, Marco; PRATT, Benjamin; THOMPSON, Aaron; TRAN, Joe; VALDEZ, Lino; (211 pag.)WO2019/168866; (2019); A1;,
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. 33348-34-4, name is 4-Amino-3-iodobenzonitrile, A new synthetic method of this compound is introduced below., category: iodides-buliding-blocks

To a round bottomed flask equipped with an addition funnel, thermometer, reflux condenser, and nitrogen inlet were added 4-cyano-2-iodoaniline (7.88 g), acetonitrile (24 ml_), and triethylamine (4.5 ml_). Trifluoroacetic anhydride (5.0 ml.) was added to the suspension while maintaining the temperature below 35-40 0C. Note: exothermic addition is addition-rate controlled. The reaction was stirred for 30 min, diluted with water (31.5 ml_). Note: initial portion of addition is exothermic and is addition-rate controlled. The slurry was held at 15-200C for 60 min. The product was isolated by filtration. The solid was washed with 80% aqueous acetonitrile, and dried in vacuo to give the title compound as a colorless solid (9.9 g); 1H NMR (300 MHz, CDCI3) delta 8.49 (1 H, br s), 8.45 (1 H, d), 8.15 (1 H, s), 7.75 (1 H, d)

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

Reference:
Patent; GLAXO GROUP LIMITED; WO2009/127678; (2009); A1;,
Iodide – Wikipedia,
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Related Products of 624-76-0, A common heterocyclic compound, 624-76-0, name is 2-Iodoethanol, molecular formula is C2H5IO, 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-Methoxy-2-methylthiopropionic acid S-(2-hydroxyethyr) ester (9); To 2.5 g (19 mmol) 8 in 20 ml of dry toluene at ice bath temperature under Ar was added 2.2 ml (14.6 mmol) DBU dropwise with stirring. Iodoethanol (1.2 ml, 14.6 mmol) in 5 ml dry toluene was added slowly to the rapidly stirred solution at O0C. The reaction mixture was then stirred for 18 hours at 5 0C. Reaction mixture was diluted with 200 ml of EtOAc and washed with 3 x 50 ml H2O. EtOAc layers were dried with Na2SO4, and solvent was removed in vacuo to give 4.7 g crude material. Silica gel chromatography with 20% EtOAc in hexanes provided 2.66 g, 79 % yield of (9). NMR 300 MHz, CDCl3, delta 3,75 (q, 2H, J=6 Hz), 3.33 (S, 3H), 3.06 (t, 2H, J=6 Hz), 2.02 (t, IH) and 1.39 (s, 6H) ppm.

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; VALEANT RESEARCH & DEVELOPMENT; WO2006/122207; (2006); A1;,
Iodide – Wikipedia,
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Synthetic Route of 58313-23-8, 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. 58313-23-8, name is Ethyl-3-iodobenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a dried sealed vessel was added 1,2,3,4-tetrahydroisoquinoline (5 mL, 40 mmol), anhydrous K2CO3 (8.34 g,60 mmol), CuI (0.8 g, 4 mmol), L-Proline (0.92 g, 8 mmol), ethyl 6-bromopicolinate (4.32 g, 20 mmol), and DMSO (25 mL). Then themixture was stirred at 80 C for 16 h under N2 environment. Aftercooling to room temperature, water (100 mL) was added andextracted with EtOAc. Then, the combined organic layer was driedover MgSO4, filtered, and concentrated. The residue was purified bysilica gel flash chromatography (hexane/EtOAc = 5/1) to providecompound 14 as a white oil (3.94 g, 70%).

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

Reference:
Article; Fang, Yuying; Zhou, Huihao; Gu, Qiong; Xu, Jun; European Journal of Medicinal Chemistry; vol. 167; (2019); p. 133 – 145;,
Iodide – Wikipedia,
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Reference of 5876-51-7, The chemical industry reduces the impact on the environment during synthesis 5876-51-7, name is 5-Iodobenzo[d][1,3]dioxole, I believe this compound will play a more active role in future production and life.

A 20 ml vial charged with 1-iodo-3,4-methylenedioxybenzene (0.13 ml, 1.001mmol), (R)-pyrrolidin-2-ylmethanol (0.11 ml, 1.115 mmol), copper (1) iodide (0.153g,0.803 mmol) and 2-propanol (3.5 ml) was evacuated and backfilled with nitrogen four times and cooled at 0C in an ice-water bath. Powdered sodium hydroxide (0.08 1 g, 2.025 mmol) was then added and the mixture was stirred for 10 minutes at 0C (solution became purple) and 16 hours at 90C (solution became orange). The reaction mixture wascooled down to room temperature, diluted with ethyl acetate, washed with water, and the water layer was back extracted twice with ethyl acetate. Combined organic layers were washed once with saturated aqueous NaHCO3 solution, once with water, once with brine, dried on anhydrous Na2SO4, filtrated and concentrated. The residue was purified on ISCO using a 25g Innoflash column (Hex/EtOAc) to give title material (0.166 g, 75%) as yellowish oil. LC (Method A): 0.886 mm. MS (APCI) calcd for C12H16N03 [M+H] rn/z 222.11, found 222.2. ?H NMR (400 MHz, acetone-d6) oe ppm 6.67 (d, J 8.2 Hz, 1 H),6.31 (d, J = 2.3 Hz, 1 H), 6.04 (dd, J = 2.5, 8.4 Hz, 1 H), 5.83 (d, J = 1.2 Hz, 1 H), 5.82 (d,J = 0.8 Hz, 1 H), 3.74 (t, J 5.7 Hz, 1 H), 3.69 – 3.58 (m, 2 H), 3.41 – 3.29 (m, 2 H), 3.02 (dt, J = 5.9, 9.0 Hz, 1 H), 2.12 – 1.87 (m, 4 H).

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, 5-Iodobenzo[d][1,3]dioxole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; UNIVERSITE DE MONTREAL; MARTEL, Alain; TREMBLAY, Francois; (207 pag.)WO2017/66863; (2017); A1;,
Iodide – Wikipedia,
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Application of 31970-26-0, 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. 31970-26-0, name is 1-(4-Iodophenyl)propan-1-one belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Finely powdered cuprous bromide (20.21 g, 91 mmol) was suspended in ethyl acetate (30 mL) and heated to reflux. A solution of ketone (14 g, 54 mmol) in chloroform (30 mL) was added dropwise over 10 minutes. After refluxing for 7 hours, the reaction was left to cool overnight and filtered through Celite. The filtrate was washed with saturated aqueous sodium bicarbonate (2¡Á50 mL) and brine (50 mL), dried over magnesium sulfate and concentrated under reduced pressure. Recrystallization from hexane afforded a pale yellow solid. mp 76 C. Yield 12.2 g (66%). 1H NMR (CDCl3) delta7.83 (d, 2H), 7.72 (d, 2H), 5.21 (q, 2H), 1.87 (d, 3H). MI=338. IR (Liq film) cm-1 1677. Calculated for C9H8BrIO: C, 31.9%, H, 2.38%. Found: C, 32.2%, H, 2.5%.

The synthetic route of 1-(4-Iodophenyl)propan-1-one has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Tisdell, Francis Eugene; Bis, Scott Jerome; Hedge, Vidyadhar Babu; Martin, Timothy Patrick; Perreault, Denise Marie; Yap, Maurice Chee Hoong; Guenthenspberger, Katherine Anne; Dripps, James Edwin; Gifford, James Michael; Schoonover, Joe Raymond; Karr, Laura Lee; Dintenfass, Leonard Paul; Neese, Paul Allen; US2004/6108; (2004); A1;,
Iodide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 627-32-7, name is 3-Iodo-1-propanol, belongs to iodides-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 627-32-7, Computed Properties of C3H7IO

To a solution of 12 (221 mg, 0.42 mmol) in MeOH (5 mL) was added KOH (26 mg, 0.46 mmol). The mixture was stirred at room temperature for 30 min, and then concentrated under reduced pressure to give a potassium salt, which was dissolved in DMF (5 mL) and treated with 3-iodo-1-propanol (52 muL, 0.55 mmol). After stirring at room temperature for 5 h, the mixture was evaporated under reduced pressure. The residue was dissolved in CH2Cl2 (20 mL) and extracted with 1 M HCl and brine. The organic phase was dried over MgSO4, concentrated under reduced pressure, and purified by flash chromatography on a silica gel column (EtOAc/hexane = 1:1) to afford ester 13 (137 mg, 55%). C28H48N4O9; colorless solid, mp 95-97 C; TLC (EtOAc/hexane = 3:1) Rf = 0.28; inlMMLBox -68.0 (c 1.4, CHCl3); IR numax (neat) 3278, 2970, 2932, 1724, 1643, 1610, 1252, 1144, 1055 cm-1; 1H NMR (400 MHz, CDCl3) delta 11.33 (1H, s), 8.58 (1H, d, J = 8.4 Hz), 6.75 (1H, s), 6.51 (1H, d, J = 8.8 Hz), 4.34-4.28 (1H, m), 4.26-4.21 (2H, m), 4.07 (1H, m), 3.97 (1H, d, J = 7.6 Hz), 3.64 (2H, t, J = 6.4 Hz), 3.29 (1H, t, J = 5.6 Hz), 2.73-2.68 (1H, m), 2.33 (1H, dd, J = 17.6, 9.2 Hz), 1.88-1.82 (5H, m), 1.50-1.43 (22H, m), 0.86-0.78 (6H, m); 13C NMR (100 MHz, CDCl3) delta 170.0, 166.0, 162.9, 156.7, 152.3, 138.4, 128.2, 83.5, 82.7, 79.5, 76.1, 61.8, 58.9, 54.3, 48.2, 31.8, 30.7, 28.4 (3¡Á), 28.1 (3¡Á), 26.1, 25.8, 23.4, 9.7, 9.4; ESI-HRMS calcd for C28H48N4O9: 585.3496, found: m/z 585.3500 [M+H]+.

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, 3-Iodo-1-propanol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Liu, Kung-Cheng; Lee, Pei-Shan; Wang, Shi-Yun; Cheng, Yih-Shyun E.; Fang, Jim-Min; Wong, Chi-Huey; Bioorganic and Medicinal Chemistry; vol. 19; 16; (2011); p. 4796 – 4802;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 76801-93-9, 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 76801-93-9 as follows.

EXAMPLE 1 ; Compound B is suspended in a mixture of acetic anhydride and acetic acid (5-15 v/v % acetic acid, about 1.5-3.0 liter of acetic anhydride and acetic acid combined per kg of Compound B) in a continuous facility as described in Figure 1. The acetylation is performed in two steps in continuous stirred tank reactors at different temperatures (55 and 120C) with residence times from about 0 to 2 hours. Excess acetic acid and acetic anhydride are removed by distillation in a continuous evaporation system. The viscous residue is diluted with methanol (which reacts with residual acetic anhydride and also with O-acetyl groups deriving from Compound B), and the resulting methyl acetate is continuously removed by atmospheric distillation at about 50-60C. The HPLC purity of the resulting crude reaction mixture is about 98 % with respect to Compound A.

According to the analysis of related databases, 76801-93-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GE Healthcare AS; EP2281814; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 41252-95-3,Some common heterocyclic compound, 41252-95-3, name is 1-Chloro-4-iodo-2-nitrobenzene, molecular formula is C6H3ClINO2, 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.

Preparation of 6-iodo-2-oxindole from 2-chloro-5-iodonitrobenzene and diethyl malonate Without Isolation of Intermediates To a jacketed reactor, N,N-dimethylacetamide (DMAc) (120 mL) and sodium ethylate (NaOEt) powder (12.1 g) is charged at 20 C. Diethylmalonate (28.8 g) is added dropwise into the above mixture while keeping internal temperature at around 10 C. After finishing addition, warm up the mixture to 20 C., and continue to stir for another 10 minutes. Then, 2-chloro-5-iodonitrobenzene (17 g) is added in one portion, and heat the mixture to 78 C. and stir for usually at least 2.5 hours until process monitor shows almost complete conversion. The resulting mixture is cooled down to 20 C., and it is quenched by 2 N cold aq. HCl solution (180 mL). The bottom yellow oil was transferred to a jacket reactor with ethanol (92 mL) in it. Then, to the above solution the first portion of SnCl2.2H2O (30 g) powder is added, and the resulting mixture is heated to 70 C. and stirred for 1 hour. The second portion of SnCl2.2H2O (30 g) is added, the mixture is stirred usually at least 0.5 hour until process monitor shows almost complete conversion. Then, heat the resulting mixture to 80 C. and add 36% aq. HCl solution (60 mL) during 0.5 hour. The mixture is stirred for at least 2.5 hours until process monitor shows almost complete conversion. Then, to the mixture water (90 mL) is added and the resulting mixture is cooled down to 20 C. Collect the solid by filtration and wash the solid with water (250 mL) to afford the crude 6-iodo-2-oxindole. Then, it is purified by crystallization with acetic acid (HOAc) (110 mL), and followed by washing with 3 N aq. HCl solution (80 mL) to afford the 6-iodo-2-oxindole in 53% yield and 99% HPLC purity (Rt=7.45 min). 1H NMR (400 MHz, DMSO) delta10.42 (S, 1H), 7.29-7.27 (dd, J=8.0, 1.6 Hz, 1H,), 7.11 (d, J=1.6 Hz, 1H), 7.02-7.00 (d, J=8.0 Hz, 1H); 13C NMR (100 MHz, CDCl3) delta 175.9, 145.3, 129.6, 126.4, 125.7, 117.4, 92.2, 35.4; MS (ESI): m/z 260.1 (M+1).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Chloro-4-iodo-2-nitrobenzene, its application will become more common.

Reference:
Patent; Boehringer Ingelheim International GmbH; SHI, Wenjian; Song, Yanli; Bao, Yuhui; Lu, Jun; Huang, Yao; Weber, Dirk; US2014/66634; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 608-28-6, name is 2-Iodo-1,3-dimethylbenzene, molecular formula is C8H9I, 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. name: 2-Iodo-1,3-dimethylbenzene

General procedure: A mixture of Cu0 powder (Sigma-Aldrich, <425mum, 99.5% trace metals basis, 0.095mg, 0.015mmol, 3-mol%), anhydrous K3PO4 (0.75mmol), 2-mercaptoimidazole/sulfur-containing azoles (0.5mmol), DMSO (0.2mL) and aryl halide (0.75mmol) were added to a reaction vial and a screw cap was fitted to it. The reaction mixture was stirred under air in a closed system at 100C for 24h. The heterogeneous mixture was subsequently cooled to room temperature and diluted with 4.0mL dichloromethane. The combined organic extracts were dried with anhydrous Na2SO4, filtered and the solvent was removed under reduced pressure. The crude product was loaded onto the column using minimal amounts of dichloromethane and was purified by silica-gel column chromatography to afford the S-arylated product. The identity and purity of products was confirmed by 1H and 13C NMR spectroscopic analys. These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 608-28-6, its application will become more common. Reference:
Article; Tan, Bryan Yong-Hao; Teo, Yong-Chua; Tetrahedron; vol. 72; 42; (2016); p. 6646 – 6653;,
Iodide – Wikipedia,
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