Category: 16932-44-8

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 16932-44-8 as follows. Safety of 2-Iodo-1,3-dimethoxybenzene

The compound (B142, 5g18.9mmol) obtained above was dissolved in the drying THF, andthe mixture obtained by adding gradually the THF solution (9.5 mL, 2.0 M19.0mmol) ofisopropyl MAGUNE SIMM chloride at 50 degree C was stirred at the room temperature for 1hour.Next, the mixture was cooled at 78 degree C, and the phosphorus trichloride (1.3 g,9.5mmol) was added slowly. Then, the reaction intermediate containing the bis(2,6dimethoxyphenyl)phosphine chloride (B-14-4) obtained by stirring all night at the roomtemperature was used for the next reaction, without refining.

According to the analysis of related databases, 16932-44-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; JAPAN POLYETHYLENE CORPORATION; JAPAN POLYPROPYLENE CORPORATION; XIN, SHIXUAN; SHIMIZU, FUMIHIKO; SATO, NAOMASA; TANNA, AKIO; (45 pag.)JP5812764; (2015); B2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 16932-44-8, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 16932-44-8 name is 2-Iodo-1,3-dimethoxybenzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

at -30 add isopropyl magnesium chloride (2.0M, 5.0mL, 10.0mmol) in THFTo compound 4 (2.64g, 10.0mmol) in anhydrous THF solution (30mL). The temperature was raised to 15 Thereafter, the mixture was stirred for 1 hour. The reaction solution was cooled to -78 , and phosphorus trichloride (0.69g,5.0mmol) were added thereto. At -78 deg.] C the resulting mixture was stirred for 1 hour. The solvent was removed under reduced pressure,To obtain a compound 5.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Iodo-1,3-dimethoxybenzene, and friends who are interested can also refer to it.

Reference:
Patent; Japan Polypropylene Corporation; Tanna, Akirahisashi; Sato, Naomasa; Konishi, Yohei; Oishi, Yasuo; (27 pag.)CN105593235; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 16932-44-8, 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 16932-44-8 as follows.

0.2 mmol of potassium carbonate, 0.005 mmol of tris (dibenzylideneacetone) dipalladium,1,3-bis (diphenylphosphine) propane 0.02mmol, 18-crown-6-ether 0.1mmol,1,3-dimethoxy-2-iodobenzene 0.1 mmol,1-phenyl-1-pentyne 0.25 mmol and1 mL of N, N-dimethylformamide was added to a 15 mL reaction tube, Repeatedly filled with nitrogen 10 times, stirred at room temperature for 15min, added 0.5mmol of water,Then placed in a reaction dish at 100 C for 16h; cooled to room temperature, the reaction solution was diluted with ethyl acetate, washed with water, the organic phase was dried over anhydrous Na2SO4, filtered, concentrated, and purified by thin layer chromatography to obtain 8.9mg of the target product Color oil, 32% yield.

According to the analysis of related databases, 16932-44-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Huaqiao University; Cheng Guolin; Lv Weiwei; (12 pag.)CN110256184; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 16932-44-8, name is 2-Iodo-1,3-dimethoxybenzene, 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 16932-44-8, category: iodides-buliding-blocks

General procedure: For a typical reaction, a Vapourtec 2R+ Series was used as the platform with a Vapourtec Gas/Liquid Membrane Reactor to load the carbon monoxide. The HPLC pump were both set at 0.125 mL/min, temperature of the reactor at 110 C, pressure of CO at 15 bar with a back pressure regulator of 250 psi (17.24 bar). The system was left running for 2 h to reach steady state after which time the flow streams were switched to pass from the loops where the substrates and catalysts were loaded. The first loop (5 mL) was filled with a solution of palladium acetate (20 mg, 0.08 mmol), triphenylphosphine (48 mg, 0.168 mmol) in 6 mL of 1,4-dioxane while the second loop (5 mL) was filled with a solution made from the ortho-substituted iodoarene substrate (1.68 mmol), triethylamine (0.272 g, 0.374 mL, 2.69 mmol) and water (0.505 g, 28 mmol) in 5.8 mL of 1,4-dioxane. An Omnifit column filled with 1.71 cm3 (r = 0.33 cm, h = 5.00 cm) of cotton was positioned just before the back pressure regulator to trap any particulate matter formed to avoid blocking of the back pressure regulator. After the substrates were passed through the system, the outlet of the flow stream was directed into a receptacle where the excess carbon monoxide gas was vented off in the fume cupboard. The reaction mixture was then evaporated to dryness, ethyl acetate (25 mL) and sodium carbonate solution (2 M, 10 mL) were added and transferred to a separating funnel. After collecting the aqueous layer, the organic layer was extracted with sodium carbonate solution (2 M, 2 × 10 mL). The combined aqueous layers were acidified by the addition of 2 M HCl solution which was then extracted with ethyl acetate (3 x 25 mL). The organic layer was dried over sodium sulfate, and the solvent evaporated under vacuum to give the crude product as a solid. The crude product was then recrystallised from the appropriate solvent.

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:
Article; Mallia, Carl J.; Walter, Gary C.; Baxendale, Ian R.; Beilstein Journal of Organic Chemistry; vol. 12; (2016); p. 1503 – 1511;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 16932-44-8, name is 2-Iodo-1,3-dimethoxybenzene, molecular formula is C8H9IO2, 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. COA of Formula: C8H9IO2

General procedure: An argon-filled flask wasadd the respective aryl halide (1.0 mmol), CuI (20 mg, 0.1 mmol, 10 mol%), L3(37 mg, 0.1 mmol, 10 mol%), KOH (168 mg, 3 mmol), thiol (1.5 mmol) and glycerol(10 mL). The contents were then stirred at 100 C for 24 h. After that, themixture was cool to room temperature, diluted with ethyl acetate (20 mL) and washedwith saturated NaCl solution (3 x 20 mL). The organic layer was separated,dried over MgSO4 and concentrated under vacuum. The crude productwas purified by flash chromatography on silica gel using hexane /ethyl acetateas eluent

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 16932-44-8, its application will become more common.

Reference:
Article; Cargnelutti, Roberta; Lang, Ernesto S.; Schumacher, Ricardo F.; Tetrahedron Letters; vol. 56; 37; (2015); p. 5218 – 5222;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 16932-44-8, 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. 16932-44-8, name is 2-Iodo-1,3-dimethoxybenzene, This compound has unique chemical properties. The synthetic route is as follows.

Example 15; 1 ) Me3SiCCH,9I (93%)[0125] 2,6-Dimethoxyphenylacetylene (91). To a stirred, degassed solution of 2-iodo-l ,3- dimethoxybenzene (13.2 g, 50 mmol), trans-dichlorobis(triphenylphosphine)palladium(II) (702 mg, 1 mmol), triphenylphospine (524 mg, 2 mmol), and copper(I) iodide (288 mg, 1.5 mmol) in 3 : 1 (v/v) toluene : diisopropylamine (200 mL) under argon is addedtrimethylsilylacetylene (8.0 mL, 57 mmol). The resulting mixture is stirred under argon at room temperature for lh, followed by 48 hour at 60C, during which period a heavy precipitate attributed to iPr2NH»HI is formed. Contents are passed on a Si02 plug with ethyl acetate as eluent. Volatiles are evaporated under reduced pressure, and the contents are passed on a short Si02 column with 95 :5 to 90: 10 pentane : ethyl acetate (v/v) as the eluent to afford the crude TMS-protected alkyne as an off-white solid that is directly carried to the next step without further purification. The solid is dissolved in THF (90 mL) and the solution is degassed by bubbling argon gas through for ca. 30 min. To the stirred mixture is added by a solution of sodium hydroxide (6 g) in methanol (30 mL). The reaction mixture is stirred at room temperature for lh, before pouring of the contents in saturated aqueous NaCl. After extration with diethyl ether and evaporation of the volatiles, the crude alkyne is purified by passage through a short Si02 column using 1 : 1 dichloromethane : pentane (v/v) as the eluent to afford alkyne 91 as a beige solid (7.55 g, 93% over 2 steps). 1H-NMR (CDC13, 300 MHz): delta = 7.25 (t, J = 8.4 Hz, 1H), 6.54 (d, J = 8.4 Hz, 2H), 3.89 (s, 6H), 3.57 (s, 1H). 13C-NMR (CDC13, 75 MHz): delta =161.9, 130.2, 103.2, 99.9, 85.3, 76.3, 55.9. Characterization data for 91 are consistent with literature values (See Wayland, B. B.; Sherry, A. E.; Poszmic, G.; Bunn, A. G. J. Am. Chem. Soc. 1992, 1 14, 1673-1681).

The chemical industry reduces the impact on the environment during synthesis 2-Iodo-1,3-dimethoxybenzene. I believe this compound will play a more active role in future production and life.

Electric Literature of 16932-44-8, 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. 16932-44-8, name is 2-Iodo-1,3-dimethoxybenzene, This compound has unique chemical properties. The synthetic route is as follows.

A mixture of 2,6-dimethoxyiodobenzene (40.1 mg, 151 mumol), Bu3SnH (48.7 muL, 181 mumol), and V-65 (7.5 mg, 30.2 mumol) in THF-d8 (4 mL) was stirred at reflux for 3 h. Bu3SnH (48.7 muL, 181 mumol) and V-65 (7.5 mg, 30.2 mumol) were added, and the mixture was stirred at reflux for 2 h. The mixture was concentrated in vacuo, and the residue was purified by column chromatography on silica gel (pentane/Et2O=40:1) to give 2-deutero-1,3-dimethoxybenzene (21.1 mg, 100%). 1H NMR (400 MHz): 3.72 (s, 6H, O-CH3), 6.46-6.51 (m, 2.15H, 2-H, 4-H, 6-H), 7.17 (t, J=8.1 Hz, 1H, 5-H); 2H NMR: 6.50 (br); MS(EI+): m/z 139 [M]+; HRMS (EI+): calcd for C8H92HO2 [M]+: 139.07436, found: 139.07515.

The chemical industry reduces the impact on the environment during synthesis 2-Iodo-1,3-dimethoxybenzene. I believe this compound will play a more active role in future production and life.

Synthetic Route of 16932-44-8, These common heterocyclic compound, 16932-44-8, name is 2-Iodo-1,3-dimethoxybenzene, 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: To a 5 mL microwave reaction tube (Biotage Inc.) equipped with a stir bar was added 21c or 21e (1 mmol), 10% Pd/C (0.04 mmol), triphenylphosphine (0.16 mmol), copper (I) iodide (0.16 mmol), trimethylsilylacetylene (1.05 mmol), triethylamine (3 mL) and acetonitrile (2 mL). The microwave tube was sealed with a crimp-cap and subjected to microwave heating in a microwave reactor (Initiator, Biotage Inc.) set at 120 C with ?fixed hold time? for 5 min. At the end of the reaction, the grey-black suspension was passed through Celite pad, washing thoroughly with hot ethyl acetate (20 mL). The filtrate concentrated in reduced pressure and silica gel (1 g) was added. Further evaporation lead to a silica gel plug which was loaded on top of a silica gel column (2 cm ¡Á 20 cm) and eluted with 5% ethyl acetate in hexanes. Fractions corresponding to the product spot were evaporated under reduced pressure to obtain an analytically pure product.

The synthetic route of 16932-44-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Gangjee, Aleem; Namjoshi, Ojas A.; Keller, Staci N.; Smith, Charles D.; Bioorganic and Medicinal Chemistry; vol. 19; 14; (2011); p. 4355 – 4365;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 16932-44-8, name is 2-Iodo-1,3-dimethoxybenzene, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 2-Iodo-1,3-dimethoxybenzene

Isopropylmagnesium chloride (10 mL, 10mmol) was added to the THF solution (60 mL) ofthe compound 1 (g [ 5.28 ], 20mmol), and it stirred at the room temperature for 1 hour. Then,the phosphorus trichloride (1.7 mL, 25mmol) was added at 78 degree C, and it stirred at theroom temperature for 2 hours. After removing a solvent and an excessive phosphorustrichloride under decompression, THF (50 mL) was added and the solution containing thecompound 2 was obtained.

According to the analysis of related databases, 16932-44-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; JAPAN POLYETHYLENE CORPORATION; JAPAN POLYPROPYLENE CORPORATION; XIN, SHIXUAN; SHIMIZU, FUMIHIKO; SATO, NAOMASA; TANNA, AKIO; (45 pag.)JP5812764; (2015); B2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 16932-44-8,Some common heterocyclic compound, 16932-44-8, name is 2-Iodo-1,3-dimethoxybenzene, molecular formula is C8H9IO2, 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: To the solution of 2 (0.125 M in THF and diethyl ether, 7.6 mL,0.95 mmol) were added a solution of 4-iodoanisole (3b, 189 mg, 0.81 mmol) in THF (1.5 mL) and Pd(PPh3)4 (17 mg, 15 mmol). After being refluxed for 6 h, the reaction mixture was filtered through a pad of silica gel (diethyl ether). The filtrate was concentrated under reduced pressure and purified by preparative thin layer chromatography on silica gel (pentane/diethyl ether = 20:1) to give 4b (119 mg, 87%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Iodo-1,3-dimethoxybenzene, its application will become more common.

Reference:
Article; Ichitsuka, Tomohiro; Takanohashi, Tsuyoshi; Fujita, Takeshi; Ichikawa, Junji; Journal of Fluorine Chemistry; vol. 170; (2015); p. 29 – 37;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com