Iodides-buliding-blocks

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. Safety of 1-Iodo-2-(2-iodoethoxy)ethane

To the mixture of sodium 2-nitrophenolate (0.5 g, 3.1 mmol) in DMF (2 mL), 1-iodo-2-(2-iodoethoxy)ethane (3 g, 9.3 mmol) is added at room temperature. The mixture is heated at 80C. for 1 hour. EtOAc (100 mL) is added at room temperature and the white precipitate is removed by filtration. The organic layer is washed with water, brine, dried (anhydrous Na2SO4) and concentrated under vacuum. The crude product is purified by silica gel column chromatography to give Compound 3 (0.9 g).

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

Reference:
Patent; AAT Bioquest, Inc.; Diwu, Zhenjun; Guo, Haitao; Peng, Ruogu; Zhao, Qin; Liao, Jinfang; Liu, Feng; (99 pag.)US9810700; (2017); B1;,
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 3718-88-5 as follows. Quality Control of 3-Iodobenzylamine hydrochloride

65 mg (0.16 mmol) of (3aS,4R,6aR)-4-(2,6-dichloropurin-9-yl)-2,2-dimethyltetrahydrothieno[3,4-d][1,3]dioxole-4-carboxylic acid methyl amide from the aforementioned Experimental Example 10, 55 mg (0.20 mmol) of 3-iodobenzylamine hydrochloride, and 0.065 mL (0.46 mmol) of triethylamine were added to ethanol and stirred at ambient temperature for 3 days. The reaction mixture was distilled under reduced pressure to obtain a concentrate. The concentrate was purified by silica gel column chromatography using the eluant (hexane:ethyl acetate=1:1) to obtain 87 mg (yield: 90%) of (3aS,4R,6aR)-4-[2-chloro-6-(3-iodobenzylamino)purin-9-yl)]-2,2-dimethyltetrahydrothieno[3,4-d][1,3]dioxole-4-carboxylic acid methyl amide as a white foam. 1H-NMR(CDCl3) delta: 1.43 (s, 3H), 1.61 (s, 3H), 2.88 (d, 3H), 3.07 (d, 2H) 4.73 (br d, 2H), 5.09 (m, 1H), 6.11 (d, 1H), 6.49 (br s, 1H), 7.07 (t, 1H), 7.32 (d, 1H), 7.60 (d, 1H), 7.72 (s, 1H), 8.16 (s, 1H) UV (methanol): lambdamax 271 nm (pH 7).

According to the analysis of related databases, 3718-88-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Government of the United States of America, repres ented by The Secretary, Department of Health and; Ewha Womans University; US2005/256143; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 51839-15-7,Some common heterocyclic compound, 51839-15-7, name is Dimethyl 5-iodoisophthalate, molecular formula is C10H9IO4, 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.

To a solution of dimethyl 5-iodoisophthalate (500 mg, 1.56 mmol, 1.0 eq) inMeOH (20 mL) was added an aqueous 1 M NaOH solution (4.69 mL, 4.69 mmol,3.0 eq). After stirring at 40 C temperature for 18 h, the brown suspension was diluted with water (10mL) and acidified to pH 3 with aqueous 1M HCl solution. The aqueous layer was extracted withEtOAc (3 x 20 mL). Combined organic extracts were washed with brine (20 mL), dried overanhydrous Na2SO4 and evaporated under reduced pressure to yield product 18 as a yellowish solid(455 mg, 100% yield), which was used in subsequent step without purification. 1H-NMR spectrumwas identical to that from the literature.9

The synthetic route of 51839-15-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zogota, Rimants; Kinena, Linda; Withers-Martinez, Chrislaine; Blackman, Michael J.; Bobrovs, Raitis; Pantelejevs, Teodors; Kanepe-Lapsa, Iveta; Ozola, Vita; Jaudzems, Kristaps; Suna, Edgars; Jirgensons, Aigars; European Journal of Medicinal Chemistry; vol. 163; (2019); p. 344 – 352;,
Iodide – Wikipedia,
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Some common heterocyclic compound, 90347-66-3, name is Methyl 3-iodo-4-methylbenzoate, 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 Methyl 3-iodo-4-methylbenzoate

A mixture of 19 (1366 mg, 4.63 mmol), (S)-tert-butyl piperidin-3-ylcarbamate (1020mg, 4.63 mmol) and K2CO3 (768 mg, 5.56 mmol) in DMF (8 mL) was stirred at roomtemperature overnight. Water was added and the mixture was extracted with EtOAc twice. Thecombined organic layers were washed with brine, dried over Na2SO4 and concentrated. Theresidue was purified by silica gel column chromatography to give 34 (870 mg, 45%) as aslightly yellow solid. LCMS (m/z: m+1): 414.0, 116.1. A suspension of 34 (870 mg, 2.1 mmol),1 (517 mg, 6.3 mmol), K2CO3 (580 mg, 4.2 mmol), CuI (120 mg, 0.63 mmol) and 8-hydroxyquinoline (61 mg, 0.42 mmol) in DMSO (8 mL) was heated at 120C overnight undernitrogen. After cooling, water was added and the mixture was extracted with EtOAc twice. Thecombined organic layers were washed with brine, dried over Na2SO4 and concentrated. Theresidue was purified by silica gel column chromatography to give 35 (630 mg, 72%) as aslightly yellow solid. LCMS (m/z: m+1): 416.3. A mixture of 35 (630 mg, 1.52 mmol) andSnCl2 2H2O (1369 mg, 6.06 mmol) in EtOH (13 ml) was heated at 80C for 1 h. After cooling,silica gel was added to the reaction and the mixture was concentrated to dryness. The residuewas purified by silica gel column chromatography to give 36 (430 mg, 74%) as a slightlyyellow solid. LCMS (m/z: m+1): 386.4. A mixture of 37 (9.5 g, 73.3 mmol), 4-fluorophenylboronic acid (10.3 g, 73.3 mmol), Na2CO3 (15.5 g, 147 mmol), and Pd(PPh3)4 (1.5g) in CH3CN/H2O (2/1, 200 mL) was heated at reflux under N2 for 16 h. After cooling, themixture was diluted with water and extracted with EtOAc twice. The combined organic layerswere washed with brine, dried over Na2SO4, filtered, concentrated and purified by silica gelcolumn chromatography to give 38 (5.1 g, 37%) as a slightly yellow solid. LCMS (m/z: m+1):190.2. A mixture of 38 (5.1 g, 27.0 mmol), 39 (11.2 g, 40.4 mmol), K2CO3 (7.5 g, 54.0 mmol),DMEDA (476 mg, 5.4 mmol) and CuI (1.28 g, 6.7 mmol) in 100 mL of dioxane was stirred at100C under N2 for 24 h. The mixture was filtered, concentrated and purified by columnchromatography to give 40 (1.6 g, 18%) as a slightly yellow solid. LCMS (m/z: m+1): 338.3.To a solution of 40 (1.6 g, 4.74 mmol) in THF/H2O (32/16 mL) was added LiOH (341 mg,14.2 mmol). The reaction was stirred at room temperature overnight and then concentrated. Tothe residue, water was added and then acidified to pH 4 with aqueous KHSO4. The precipitatewas filtered and washed with water and EtOAc. The cake was collected and dried to give 41(1.3 g, 85%) as an off-white solid. LCMS (m/z: m+1): 324.1. A mixture of 36 (130 mg, 0.34mmol), 41 (109 mg, 0.34 mmol), HATU (257 mg, 0.68 mmol) and DIEA (218 mg, 1.69 mmol)in DMF (2 mL) was heated at 70C overnight. After cooling, the reaction mixture was directlypurified by reverse prep-HPLC and then silica gel prep-TLC to give 42 (33 mg, 14%) as aslightly yellow solid. LCMS (m/z: m+1): 691.3. To a solution of 42 (33 mg, 0.048 mmol) inCH2Cl2 (2 mL) was added TFA (1 mL) and the reaction was stirred at room temperature for 4h before being concentrated under reduced pressure. The residue was treated with water,basified with 0.5 N NaOH and extracted with CH2Cl2/MeOH (15/1) 3 times. The combinedorganic layers were dried over Na2SO4, filtered, concentrated and purified by reverse prep-HPLC to give 2a (14 mg, 50%) as an off-white solid.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 90347-66-3, its application will become more common.

Reference:
Article; Bonnar, James; Dixon, Ian; Evison, Benny J.; Kelly, Graham E.; Kumar, Sanjay; Lambert, Gilles; Nativel, Brice; Palmer, James T.; Parmar, Jasneet; Rathi, Anuj Kumar; Suchowerska, Alexandra K.; Tang, Wei; Teng, Yanfen; Treutlein, Herbert; Wang, Jie; Xu, Yanfeng; Zeng, Jun; Zhu, Qing; Chemello, Kevin; Bioorganic and medicinal chemistry; vol. 28; 6; (2020);,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 672293-33-3, name is Methyl 4-amino-5-iodo-2-methylbenzoate, A new synthetic method of this compound is introduced below., Quality Control of Methyl 4-amino-5-iodo-2-methylbenzoate

To a solution of methyl 4-amino-5-iodo-2-methylbenzoate 2 (0.84 g, 2.90 mmol, 1 eq.) in DMF (10 mL), 2-oxobutyric acid (1.48 g, 14.5 mmol, 5 eq.) and DABCO (0.975 g, 8.7 mmol, 3 eq.) were added. The solution was stirred for 5 min and then palladium (II) diacetate (0.03 g, 0.145 mmol, 0.05 eq.) was added. The mixture was warmed to 105C, stirred during 16 h and then concentrated. The resulting solid was dissolved in AcOEt (150 mL) and washed with water (150 mL). The organic layer was dried over anhydrous Na2SO4 and concentrated in vacuuo to obtain dark brown solid which was purified by trituration in AcOEt to give the desired indole 6 as grey powder (358 mg, 1.45 mmol, 50%); Mp : 280-282C (Dec.); Rf = 0.61 (SiO2, Cyc/AcOEt, 5/5); 1H NMR (400 MHz, CD3OD) 8.30 (s, 1H, H-4), 7.25 (s, 1H, H-7), 3.99 (s, 3H, CH3), 2.65 (s, 3H, CH3), 2.59 (s, 3H, CH3); 13C NMR (100 MHz, CD3OD) 168.1 (C=O), 165.3 (C=O), 139.6 (C), 137.2 (C), 128.0 (C), 127.7 (C), 125.6 (CH), 122.3 (C), 118.9 (C), 114.8 (CH), 52.1 (CH3), 22.9 (CH3), 9.94 (CH3); HR-ESIMS: [M-H]- m/z calcd for C13H12NO4 246.0766 found 246.0777.

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; Vogrig, Alexandre; Boucherle, Benjamin; Deokar, Hemantkumar; Thomas, Isabelle; Ripoche, Isabelle; Lian, Lu-Yun; Ducki, Sylvie; Bioorganic and Medicinal Chemistry Letters; vol. 21; 11; (2011); p. 3349 – 3353;,
Iodide – Wikipedia,
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These common heterocyclic compound, 51839-15-7, name is Dimethyl 5-iodoisophthalate, 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. Application In Synthesis of Dimethyl 5-iodoisophthalate

Step A and B: Cross-coupling and Saponification. To a solution of dimethyl 5-iodoisophthalate (13 g, 40.6 mmol) in 100 mL THF was added 2-cyano-phenyl zinc bromide (97.5 mL, 48.7 mmol, 0.5 M THF) and tetrakis(triphenylphosphine) palladium (214 mg, 0.2 mmol) and the reaction mixture was stirred at room temperature for 2 h. The precipitated solid was filtered, the filtrate was diluted with MeOH to provide after filtration a second crop for a total of 10.1 g of dimethyl 5-(2-cyanophenyl)isophthalate which was hydrolyzed to the corresponding monoacid 2′-cyano-5-(methoxycarbonyl)-1,1′-biphenyl-3-carboxylic acid following a similar procedure as described in intermediate B preparation, step C: 1H NMR (400 MHz, d6-DMSO) delta 13.55 (br s, 1H), 8.60-8.55 (m, 1H), 8.38-8.31 (m, 2H), 8.02 (d, J=8.3 Hz, 1H), 7.85 (td, J=8.3 Hz, 1.5 Hz 1H), 7.75 (d, J=8.3 Hz, 1H), 7.66 (td, J=8.3 Hz, 1.5 Hz 1H), 3.93 (s, 3H).

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

Reference:
Patent; Barrow, James C.; Coburn, Craig A.; Nantermet, Philippe G.; Selnick, Harold G.; Stachel, Shawn J.; Stanton, Matthew G.; Stauffer, Shaun R.; Zhuang, Linghang; Davis, Jennifer R.; US2007/142634; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 6213-88-3,Some common heterocyclic compound, 6213-88-3, name is (E)-Methyl 3-iodoacrylate, molecular formula is C4H5IO2, 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.

Method 1: To a dry Schlenk flask was added Pd(OAc)2 (36 mg,0.16 mmol), P(o-tol)3 (0.10 g, 0.33 mmol) and AgOAc (0.601 g,3.60 mmol). The flask was purged with argon, and dry, degassed MeCN (10 mL) was added. 4,4,6-Trimethyl-2-vinyl-1,3,2-dioxaborinane (0.655 mL, 3.80 mmol) was then added, followed by methyl (2E)-3-iodoprop-2-enoate (0.704 g, 3.32 mmol). The vessel was purged further with argon, and the reaction mixture was then heated to 50 C with vigorous stirring for 2 days. The mixture was allowed to cool, then diluted with Et2O (280 mL) and passed through a short Celite/silica plug. The organic extracts were washed with 5% HCl (40 mL), H2O (80 mL) and brine (80 mL), dried over MgSO4, filtered and evaporated to yield 0.98 g of crude product as an orange oil. The crude product was purified by silica gel chromatography, eluent 10% EtOAc in hexane elution. Pure fractions were evaporated to yield (2E,4E)-5-(4,4,6-trimethyl-[1,3,2-dioxaborinan-2-yl]-penta-2,4-dienoic acid methyl ester as a yellow oil (0.404 g, 51%). 1H NMR (400 MHz, CDCl3): delta 1.35-1.24 (9H, m), 1.5-1.47 (1H, m), 1.81 (1H, dd, J = 14.0, 2.9 Hz), 3.75 (3H, s), 4.24 (1H, dqd, J = 12.3, 6.2, 2.9 Hz), 5.99-5.86 (2H, m), 6.97 (1H, ddd, J = 17.3, 11.0, 0.7 Hz), 7.33-7.21 (1H, m); 11B NMR (128 MHz, CDCl3): delta 25.52; 13C NMR (101 MHz, CDCl3): delta 23.58, 28.62, 31.65, 46.41,52.12, 65.52, 71.67, 123.17, 143.89, 146.54, 167.93; IR (upsilonmax, cm-1) 2974.3 (w) 1719.5 (s) inter alia; LCMS (ESI) 239.2; HRMS (ESI) calculated [C12H19BO4H] 238.1470, found 238.1491. Method 2: To a dry flask was added methyl (2E)-3-iodoprop-2-enoate (2.82 g, 13.3 mmol), Pd(OAc)2 (0.150 g, 0.67 mmol), P(otol)3 (0.408 g, 1.34 mmol) and AgOAc (2.41 g, 14.4 mmol). The flask was purged with argon, and dry, degassed MeCN (80 mL) wasadded. 4,4,6-Trimethyl-2-vinyl-1,3,2-dioxaborinane (2.6 mL,15 mmol) was then added, the vessel was purged further with argon, and the reaction mixture was then heated to 50 C with vigorous stirring for 23h. The mixture was allowed to cool, then diluted with Et2O (200 mL) and passed through a short Celite/silicaplug. The organic extracts were washed with NH4Cl (200 mL), H2O(200 mL) and brine (200 mL), dried over MgSO4, filtered and evaporated to give crude product as a yellow oil (2.65 g, 83%). The compound was taken on to the next stage without any further purification or characterisation. Method 3: To a dry flask was added methyl (2E)- 3-iodoprop-2-enoate (2.82 g, 13.3 mmol), Pd(OAc)2 (0.15 g, 0.67 mmol), P(o-tol)3(0.408 g, 1.34 mmol) and AgOAc (2.41 g, 14.4 mmol). The flask was purged with argon, and dry, degassed MeCN (72 mL) was added. 4,4,6-Trimethyl-2-vinyl-1,3,2-dioxaborinane (2.6 mL, 15 mmol) was then added, the vessel was purged further with argon, and the reaction mixture was then heated to 30 C with vigorous stirring for 19 h. The mixture was allowed to cool, then diluted with Et2O (200 mL) and passed through a short Celite/silica plug. The solvent was evaporated to give crude product as a yellow oil (2.84 g, 89%).The compound was taken on to the next stage without any further purification or characterisation. Method 4: To a dry flask was added methyl (2E)-3-iodoprop-2-enoate (1.0 g, 4.7 mmol), Pd(OAc)2 (0.011 g, 0.047 mmol), tri(2-furyl)phosphine (0.022 g, 0.094 mmol) and AgOAc (0.851 g, 5.11 mmol). The flask was purged with argon, and dry, degassed MeCN (28 mL) was added. 4,4,6-Trimethyl-2-vinyl-1,3,2-dioxaborinane (0.93 mL, 5.4 mmol) was then added, the vessel was purged further with argon, and the reaction mixture was stirred vigorously at room temperature for 3 days. The mixture was diluted with Et2O (71 mL) and passed through a short Celite/silica plug. The solvent was evaporated to give crude product as a pale yellow oil (1.18 g, 99%). The compound was taken on to the next stage without any further purification or characterisation.

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

Reference:
Article; Madden, Katrina S.; Knowles, Jonathan P.; Whiting, Andrew; Tetrahedron; vol. 75; 45; (2019);,
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. 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene, This compound has unique chemical properties. The synthetic route is as follows., Safety of 4-Bromo-1-iodo-2-nitrobenzene

Intermediate M2-b (4.8 g, 15 mmol), 2-iodo-5-bromonitrobenzene (5.9 g, 18 mmol),Sodium tert-butoxide (2.9 g, 30 mmol), 50 mL of toluene, protected with nitrogen,0.17 g of d2(dba)3, tri-tert-butylphosphine (11 ml, 10% in toluene),The stirring was started, and the mixture was heated to reflux at 100 C for 12 hours.The reaction solution is washed with water, and the organic phase is concentrated and passed through a silica gel column.The eluent is petroleum ether: ethyl acetate = 50:1, concentrated eluent,Obtaining intermediate M2-c(6.6 g, yield 84.6%).

According to the analysis of related databases, 112671-42-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Beijing Dingcai Technology Co., Ltd.; Gu’an Dingcai Technology Co., Ltd.; Fan Hongtao; Zhang Yaguang; Zhang Xianghui; Ren Xueyan; (39 pag.)CN108341824; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 1219741-79-3, name is 4-Bromo-5-fluoro-2-iodoaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 4-Bromo-5-fluoro-2-iodoaniline

To a vial was added, 4-bromo-5-fluoro-2-iodoaniline (5.67 g, 17.95 mmol), PdOAc2 (0.201 g, 0.897 mmol), sodium bicarbonate (3.77 g, 44.9 mmol), ethyl acrylate (2.049 ml, 18.85 mmol) and DMF (12.0 ml). The reaction was heated for 3 hour at 100 C. The reaction was cooled to RT, diluted with water and extracted with DCM (3*). The combined organics were washed with water and brine, dried over magnesium sulfate, filtered and concentrated. The resulting material was triturated with heptane overnight and then filtered to afford (E)-ethyl 3-(2-amino-5-bromo-4-fluorophenyl)acrylate (4.00 g, 13.88 mmol, 77% yield) as a light yellow solid. m/z (ESI) 288.0 (M+H)+.

The synthetic route of 1219741-79-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Amgen Inc.; Weiss, Matthew; Boezio, Alessandro; Boezio, Christiane; Butler, John R.; Chu-Moyer, Margaret Yuhua; Dimauro, Erin F.; Dineen, Thomas; Graceffa, Russell; Guzman-Perez, Angel; Huang, Hongbing; Kreiman, Charles; La, Daniel; Marx, Isaac E.; Milgrim, Benjamin Charles; Nguyen, Hanh Nho; Peterson, Emily; Romero, Karina; Sparling, Brian; US9212182; (2015); B2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 52807-27-9,Some common heterocyclic compound, 52807-27-9, name is 4-Chloro-2-iodoanisole, molecular formula is C7H6ClIO, 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.

4-Chloro-2-iodophenol; 109.4g (0.436mol) of boron tribromide were added over 10 minutes to a stirred solution of 9Og (0.335mol) of 4-chloro-2-iodoanisole in dichloromethane (900ml) at -780C under nitrogen. Cooling was removed and allowed to warm to room temperature and stirred for 5 hours. Poured onto ice and diluted with a further 800ml of water. The organic phase was separated, the aqueous extracted with dichloromethane and the combined organics washed with saturated sodium bicarbonate, dried and evaporated to give 84.87g of off- white solid; Sodium 6-r(5-chloro-2-fr(4-chloro-2-fluorophenyl)methvnoxy)phenyl)methvn-2- pyridinecarboxylate (Alternative route 2); 4-Chloro-2-iodophenol; Boron tribromide (1349g) was added to a solution of 4-chloro-2-iodoanisole (1025g) in dichloromethane (10.3L) under nitrogen at such a rate that the temperature remained at 0- 5C The solution was then warmed to 200C and stirred for c. 19h until the reaction was complete by HPLC. This organic solution was added to water (8.2L) and the mixture was cooled to 5C to 10C. DCM (770ml) was added and the resuting biphasic mixture was then stirred at 50C for 15 min before being warmed to 220C and then finally stirred at 22C for 20 min before separating the phases. The separated organic phase was washed with aqueous saturated sodium bicarbonate (3.1L), water (3.1L) and then evaporated on a Buchi to give the title compound. (963.6g)

The synthetic route of 52807-27-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; WO2006/66968; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com