Tag: M.W=300-400

These common heterocyclic compound, 98-61-3, name is 4-Iodobenzenesulfonyl chloride, 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. Formula: C6H4ClIO2S

General procedure: A: Sulfonyl chloride (1 eq.) was dissolved in a mixture of dry DCM (0.2 M) and TEA (1.5 eq.). Amine (1.2 eq.) was added and the reaction was stirred at 20 C until completion (TLC). The solvent was removed under reduced pressure and the crude product was purified by column flash-chromatography on silica to give the sulfonamide.

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

Reference:
Article; Heinrich, Daniel M.; Flanagan, Jack U.; Jamieson, Stephen M.F.; Silva, Shevan; Rigoreau, Laurent J.M.; Trivier, Elisabeth; Raynham, Tony; Turnbull, Andrew P.; Denny, William A.; European Journal of Medicinal Chemistry; vol. 62; (2013); p. 738 – 744;,
Iodide – Wikipedia,
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Related Products of 811842-30-5, These common heterocyclic compound, 811842-30-5, name is 2-Bromo-1-fluoro-4-iodobenzene, 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.

Mix 2-bromo-1-fluoro-4-iodobenzene (18.0 g, 0.06 mol), Cu2O (36.0 mg, 0.25 mmol), and KOH (5.6 g, 0.10 mol) in 1,4-dioxane (20 ml) ), Under the protection of nitrogen, cyclopentathiol (5.1 g, 0.05 mol) was added to the system through a syringe, and the temperature was raised to 110 C. for overnight reaction. After the reaction solution was cooled to room temperature, ethyl acetate (30 ml) was added, and the filter cake was washed with ethyl acetate (20 ml). The filtrates were combined and concentrated to dryness under reduced pressure. The residue was separated by column chromatography to obtain the title compound (12.0 g, yield 72%).[1283]1H NMR (400MHz, CDCl 3) delta 7.62-7.49 (m, 1H), 7.34-7.20 (m, 1H), 7.09-6.95 (m, 1H), 3.52 (td, J = 7.2, 3.6Hz, 1H) , 2.08–1.92 (m, 2H), 1.85–1.56 (m, 6H).

The synthetic route of 811842-30-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JIANGSU HANSOH PHARMACEUTICAL GROUP CO., LTD.; SHANGHAI HANSOH BIOMEDICAL CO., LTD.; SU, Yidong; GU, Peng; CHEN, Xiaopo; LIU, Lei; BAO, Rudi; (192 pag.)WO2018/130174; (2018); A1;,
Iodide – Wikipedia,
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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. 755027-18-0, name is 1-Bromo-4-iodo-2-methoxybenzene, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C7H6BrIO

1-Bromo-4-iodo-2-methoxybenzene (50 g, 160 mmol) was suspended in CH2CI2 (75 mL) at -10 C. Boron tribromide (250 mL, 250 mmol, 1M in CH2CI2,) was cannulated in over 30 min, with the internal temperature remaining below 0 C throughout the addition. After the addition, the mixture was stirred at 0C for 1 hour, and then at room temperature for 16 hours. The mixture was cooled in an ice bath. 10% Aqueous Na2C03 (250 mL) was added in portions. The mixture was then partitioned between H20 and CH2Cl2. The CH2Cl2 layer was dried over MgS04 and then filtered. 2-Bromo-5-iodophenol (46 g, 96%) was obtained from the filtrate as a pinkish-white solid. 1H NMR (acetone-< d: 9.24 (br s, 1H), 7.38 (d, 7=2 Hz, 1H), 7.31 (d, 7=8.5 Hz, 1H), 7.17 (dd, 7=8.5 Hz, 2 Hz, 1H). Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 755027-18-0. Reference:
Patent; PTC THERAPEUTICS, INC.; CHEN, Guangming; BHATTACHARYYA, Anuradha; JIANG, Yao; KARP, Gary, Mitchell; NARASIMHAN, Jana; TURPOFF, Anthony; ZHANG, Nanjing; (0 pag.)WO2020/5882; (2020); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 19821-80-8, 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. 19821-80-8 name is 1,3-Dibromo-2-iodobenzene, 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 -75 C butyllithium (14 mmol) in hexanes (5.6 mL) was added to a solution of 1,3-dibromo-2-iodobenzene (4.3 g, 12 mmol) in diethyl ether (0.18 L). After the solution was stirred for 2 h at -75 C, copper(II)chloride (9.7 g, 72 mmol) was added, and the reaction mixture was allowed to attain 25 C over a 12 h period. Cold water was added to the reaction mixture and the organic layer was separated. The aqueous phase was extracted with ethyl acetate (2×0.10 L). The combined organic layers were dried over sodium sulfate before being evaporated. 2,2′,6,6′-tetrabromo-1,1′-biphenyl precipitates upon treatment of the residue with hexanes cooled to -20 C. The product is pure enough for further reaction; m.p. 214 – 215 C; 9.0 g (33%);1H NMR (CDCl3, 400 MHz): delta = 7.67 (d, J= 8.3 Hz, 4 H), 7.17 (t, J = 8.0 Hz, 2 H).

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

Reference:
Patent; Lonza AG; EP1609795; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 16355-92-3, name is 1,10-Diiododecane, 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. Quality Control of 1,10-Diiododecane

A mixture of 4-aminoquinaldine 4 kg (25.3 mol),Bis-iodide decane4.3 kg (10.9 mol),Nitrobenzene 9L into the reaction tank,Stir,Heating to 150-160 C,Maintain the temperature reaction for 6 hours,Cooled to room temperature,filter,Respectively, washed twice with methanol (4L each),Filter dry,Washed with 5% hydrochloric acid solution twice,Washed with water to pH 6,Filter dry,And then rinse with the amount of methanol once,Filter dry,60-70 drying,Get grayish yellow powder,That is, decane 1,10-bis (4-aminoquinaldin iodide) salt (referred to as quaternary ammonium iodide).The yield of quinacridine was 3.64 kg,Yield of about 47%.After testing,The quaternary ammonium iodide has a melting point of 300-308 C.

The synthetic route of 1,10-Diiododecane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; (12 pag.)CN106854179; (2017); A;,
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. 4897-68-1, name is 1-Bromo-2-iodo-4-methoxybenzene, A new synthetic method of this compound is introduced below., Product Details of 4897-68-1

Example 1 Synthesis of 2-bromo-4-methoxybiphenyl A mixture of 38 g (121 mmol) of 1-bromo-2-iodo-4-methoxy benzene, 14.8 g (121 mmol) of phenylboronic acid, 2.8 g (2.4 mmol) of tetrakis(triphenylphosphine)palladium, 2M Na2CO3 (29 g, 266 mmol), 135 ml of EtOH and 270 ml toluene was degassed and placed under nitrogen, and then heated at 90 C. for 16 h. After finishing the reaction, the mixture was allowed to cool to room temperature. The organic layer was extracted with ethyl acetate and water, dried with anhydrous magnesium sulfate, the solvent was removed and the residue was purified by column chromatography on silica(hexane-dichloromethane) to give product (24 g, 63.0 mmol, 75%).

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; Luminescence Technology Corp.; YEN, FENG WEN; CHANG, CHENG HAO; TENG, CHIN MIN; LIN, I FENG; (46 pag.)US2016/155949; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference 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,
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. 83027-73-0, name is 5-Bromo-1-chloro-3-fluoro-2-iodobenzene, A new synthetic method of this compound is introduced below., Quality Control of 5-Bromo-1-chloro-3-fluoro-2-iodobenzene

Dry methanol (160 mL) was cooled to 10 C and potassium hydroxide (14.9 g) was added portion wise over 25 minutes. Once dissolved, this solution was added over 15 minutes to a refluxing solution of 5-bromo-1-chloro-3-fluoro-2-iodo-benzene (CAS 83027-73-0, 40.0 g) in dry methanol (320 mL). After 46 hours refluxing the reaction mixture was concentrated and partitioned between water (500 mL) and ethyl acetate (500 mL). The aqueous phase was extracted with further ethyl acetate (2 x 200 mL). The combined organic layers were washed with brine (400 mL), dried over magnesium sulfate, concentrated and purified by chromatography on silica eluting with ethyl acetate in iso-hexane to give 5-bromo-1-chloro-2- iodo-3-methoxy-benzene (37.767 g) as a pale pink solid 1H NMR (500 MHz, CDCI3) 7.28 (d, 1 H), 6.82 (d, 1 H), 3.90 (s, 3H).

The synthetic route of 83027-73-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SYNGENTA LIMITED; MOUND, William Roderick; SCUTT, James Nicholas; SLATER, Mark; WILLETTS, Nigel James; WO2014/96289; (2014); A2;,
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. 450412-28-9, name is 1-Bromo-3-chloro-2-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 450412-28-9

A sdution of 5-(44,5,5-tetramethy-1 32-doxabordan-2-yndohn-2-one (250 mg, 0.96 mmd), 1-bromo-3-choro-2-odobenzene (373mg, 1.2 mmd), and potassum phosphate (410 mg, 1.9 mmd) n 4:1 doxane: water (3.0 rnL) was degassed with n[trogen for 10 minutes. PdC2(dppf)-CH2C2 (35 mg, 0.05 mmd) was added at once and the resuWng mixture was degassed w[th n[trogen for an add Wona 10 minutes. The reacUon rnxturewas heated at 100 C for 16 h. After coohng to rt, water was added and the aqueous ayer was extracted w[th DCM (x3). The combined orgadc extracts were dried over Na2SO4 and concentrated n vacuo. Purflcafion (FCC, SO2; 0 50% EtOAc/hexanes) provided the tWe compound as a white sohd (189 mg, 61% yed). MS (ES): mass cacd. for C14H9BrCNO, 321.0; rn/z found. 321.9 [M+Hj. 1H NMR (500 MHz, DMSO-d6) oe 10.50 (5,IH), 772(dd, J=8.1, 1.1 Hz, IH), 760 (dd, J=8.1, 1.1 Hz, IH), 7.32(t, J=8.1 Hz, IH),7.11 -6.97 (m, 2H), 6.91 (dd, J=8.0, 0.6 Hz, IH), 353 (5, 2H).

According to the analysis of related databases, 450412-28-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; AMERIKS, Michael K.; RAVULA, Suchitra; SAVALL, Bradley M.; SWANSON, Devin M.; ZIFF, Jeannie M.; SHIREMAN, Brock T.; (167 pag.)WO2016/176463; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 1133123-02-0, 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. 1133123-02-0, name is 4-Bromo-2-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Under argon, 0.79 g of lithium hydroxide was added to a 250 mL two-neck reactor,50 mL of N-methylpyrrolidone and water were added,4.89 g of 2-iodo-4-bromobenzoic acid and 2 g of phenylboronic acid were added,Add triacetylacetone dipalladium chloride adduct with stirring.Followed by stirring at 65 C for 18 hours. After completion of the reaction, hydrochloric acid was added,Extracted with methyl tert-butyl ether, separated,The organic phase was dried over anhydrous sodium sulfate and the organic liquid was removed by distillation. The product was purified by column chromatography using petroleum ether.And dried to give 4-bromo-2-phenylbenzoic acid as a white powder (yield: 2.9 g, yield: 70.5%).

The synthetic route of 4-Bromo-2-iodobenzoic acid has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Soochow University (Suzhou); Zhang Xiaohong; Chen Jiaxiong; Zheng Caijun; (11 pag.)CN106699747; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com