Month: March 2021

Synthetic Route of 74534-15-9, 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. 74534-15-9, name is 1-Chloro-2-iodo-4-nitrobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The appropriate product 2 (1 mmol, 1 eq) in AcOH/EtOH (1:1, 0.42 M) was added slowly to a solution of Iron powder (6 eq) in AcOH/EtOH(1:2, 2 M) at 60C . The solution was stirred at 70C for 30-60 mins. The reaction mixture was cooled to 23C , filtered through celite, washed with ethyl acetate, and concentrated. The oily residue was dissolved in ethyl acetate (30 mL), washed with saturated aq. NaHCO3 (1 x 15 mL), water (2 x 10 mL), dried (MgSO4) and concentrated. The oily residue was used without further purification.

The synthetic route of 1-Chloro-2-iodo-4-nitrobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wang, Fangying; Jiang, Hongxia; Deng, Yufang; Yu, Jiang; Zhan, Miao; Zhao, Lifeng; Chen, Yuanwei; Bioorganic and Medicinal Chemistry Letters; vol. 28; 14; (2018); p. 2399 – 2402;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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 573764-31-5 as follows. Recommanded Product: 573764-31-5

3) Preparation of 4-chloro-3-(4,4,5,5,-tetramethyl-1,3,2-dioxaborolan-2-yl)aniline (compound 1-5) A mixture of compound 1-4 (10 g, 39.5 mmol), 4,4,4′,4′,5,5,5′,5′-octamethyl-2,2′-bi(1,3,2-dioxaborolane) (20.0 g, 79.0 mmol), KOAc (11.6 g, 118.5 mmol), and PdCl2(dppf) (960 mg, 1 mmol) in 1,4-dioxane (60 mL) was stirred at 105¡ã C. for 8 h under N2. The reaction mixture was concentrated in vacuo, and the residue was purified by column chromatography (hexanes/dichloromethane: 3/1 to 1/1) to afford compound 1-5 as a light yellow solid (6.0 g, 60percent yield). LCMS: m/z 295.1 [M+42]+. 1H NMR (400 MHz, CDCl3): delta 1.36 (s, 12H), 3.61 (br, 2H), 6.65 (dd, J=8.8 Hz, 2.8 Hz, 1H), 7.00 (d, J=2.8 Hz, 1H), 7.11 (d, J=8.8 Hz, 1H).

According to the analysis of related databases, 573764-31-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Genetech, Inc.; Curis, Inc.; Cai, Xiong; Qian, Changgeng; Zhai, Haixiao; US2014/18368; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 181765-86-6, A common heterocyclic compound, 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, molecular formula is C8H6BrIO2, 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.

500mL round-bottom flask reactor, methyl 5-bromo-2-iodo benzoate (25.0g, 73mmol) in 4-dibenzofuran boronic acid [0410] (18.7g, 88mmol), tetrakis (triphenylphosphine) palladium (1.7g, 0.15mmol), potassium carbonate (20.2 g, 146.7mmol) put the toluene 125 mL, tetrahydrofuran 125mL, water 50 mL. The temperature of the reactor was 80 C, 10 hours was stirred. When the reaction is complete cool down the temperature of the reactor to room temperature, extracted with ethyl acetate and the organic layer was separated It was. The organic layer was concentrated under reduced pressure and separated by column chromatography to give the intermediate 1-a. (75.0g, 60.1%)

The synthetic route of 181765-86-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SFC CO LTD; PARK, SEOK BAE; SONG, JU MAN; LEE, YUR IM; KIM, HEE DAE; PARK, SANG WOO; JEONG, KYUNG SEOK; CHA, SOON WOOK; (96 pag.)KR2015/130206; (2015); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. Application In Synthesis of 1-Bromo-4-iodo-2-methoxybenzene

To a solution of 2-bromo-5-iodoanisole (400 mg, 1.28 mmol) in tetrahydrofuran (5 mL) at -78 C. was added n-butyl lithium (2.5 M in hexane, 0.62 mL, 1.55 mmol) dropwise over 15 minutes. The reaction mixture was stirred at -78 C. for 30 minutes, then treated with neat cyclobutanone (0.1 mL, 1.3 mmol) dropwise over 10 minutes and stirred at -78 C. for an additional 1.5 hours. The reaction was quenched with saturated aqueous ammonium chloride solution, warmed to room temperature and extracted with ethyl acetate (2*). The combined organic layers were dried over magnesium sulfate, filtered and concentrated in vacuo to afford a yellow oil, which was purified by flash chromatography (12 g silica, 0-50% ethyl acetate/heptane, 27 column volumes). Product fractions were combined and concentrated in vacuo to afford the title compound as a pale yellow oil (40 mg, 12% yield). GCMS 256/258 (M)+; 1H NMR (500 MHz, CDCl3) delta 7.53 (d, J=8.29 Hz, 1H), 7.09 (d, J=1.95 Hz, 1H), 6.98 (dd, J=8.17, 1.83 Hz, 1H), 3.94 (s, 3H), 2.51-2.61 (m, 2H), 2.35-2.46 (m, 2H), 2.02-2.10 (m, 1H), 1.66-1.79 (m, 1H).

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; PFIZER INC.; Bhattacharya, Samit; Cameron, Kimberly; Dowling, Matthew; Fernando, Dilinie; Ebner, David; Filipski, Kevin; Kung, Daniel; Lee, Esther; Smith, Aaron; Tu, Meihua; US2013/267493; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 167479-01-8, 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. 167479-01-8, name is tert-Butyl (3-iodopropyl)carbamate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a solution of an aminoalcohol (66.6 mmol) in THF (67 mL) was added di-tert-butyl dicarbonate (15.3 g, 66.6 mmol) at 50 C under an argon atmosphere. After 3 h stirring, the solvent was removed in vacuo. The crude product was purified by silica gel column chromatography (EtOAc / hexane, 50:50) to give a N-Boc aminoalcohol. Iodine (12.5 g, 49.3 mmol) was added to a solution of N-Boc aminoalcohol (17.6 mmol), PPh3 (6.92 g, 26.3 mmol) and imidazole (1.79 g, 26.3 mmol) in CH2Cl2 (98 mL) at 0 C. The mixture was stirred at room temperature for 1 h under an argon atmosphere. The reaction mixture was quenched with saturated aqueous Na2S2O3, diluted with CH2Cl2 and extracted with CH2Cl2. The organic layer was washed with H2O and brine, dried over MgSO4, filtered and concentrated in vacuo. The residue was purified by silica gel column chromatography (EtOAc/hexane, 10:90) to afford a N-BOC aminoalkyliodide. To a solution of NaH (60% in oil, 0.673 g, 16.8 mmol) in DMF (15.3 mL) was added dropwise a solution of N-hydroxyphthalimide (2.49 mmol) in DMF (10 mL) at 0 C under an argon atmosphere. After 15 min of stirring, a solution of the iodide (15.3 mmol) in DMF (10 mL) was added dropwise to the solution and stirred at 70 C for 12 h. After cooled to 0 C, the reaction was quenched with H2O and filtrated to afford colorless solid, which was recrystallized to give a N-alkoxyphthalimide 13a-d.

The synthetic route of tert-Butyl (3-iodopropyl)carbamate has been constantly updated, and we look forward to future research findings.

Reference:
Article; Fukuda, Hiroshi; Nishikawa, Keisuke; Fukunaga, Yukihiro; Okuda, Katsuhiro; Kodama, Kozue; Matsumoto, Kenji; Kano, Arihiro; Shindo, Mitsuru; Tetrahedron; vol. 72; 41; (2016); p. 6492 – 6498;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 112671-42-8,Some common heterocyclic compound, 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene, molecular formula is C6H3BrINO2, 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) Add 42g (100mmol) of M3 to the reaction flask,2-iodo-5-bromonitrobenzene (110mmol),Tetratriphenylphosphine palladium 0.9g (0.785mmol, 0.5%),500mL of toluene, 200mL of ethanol,200mL of water and 40g (300mmol) of potassium carbonate, react at 100 for 8h;After the reaction is complete, stop the reaction; cool to room temperature, concentrate, and silica gel column chromatography to obtain white powder M4;

The synthetic route of 112671-42-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Yantai Xianhua Chemical Technology Co., Ltd.; Xing Qifeng; Feng Peichuan; Chen Yue; Hu Lingfeng; Chen Yili; (27 pag.)CN111004241; (2020); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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 103962-05-6 as follows. Recommanded Product: 1-Iodo-4-(trifluoromethoxy)benzene

General procedure: A dry and argon-flushed Schlenk-flask, equipped with a magnetic stirring bar and a rubberseptum, was charged with FeCl2 (10 molpercent, 99.5percent pure), the corresponding electrophile (1.0equiv) and freshly distilled THF. Thereupon, the benzylic manganese(II) chloride solution (1.05-1.10 euqiv) was dropwise added at 0 ¡ãC. After the addition was complete, the reaction mixturewas stirred for a given time at the prior adjusted temperature and then allowed to warm toroom temperature. The reaction completion was monitored by GC-analysis of quenched aliquots.A saturated aqueous solution of NH4Cl was added and the aqueous layer was extracted threetimes with Et2O or EtOAc (3 ¡Á 50 mL). The combined organic layers were dried over MgSO4,filtered and concentrated under reduced pressure. Purification of the crude products by flashcolumn chromatography afforded the desired products.

According to the analysis of related databases, 103962-05-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Benischke, Andreas D.; Breuillac, Antoine J. A.; Moyeux, Alban; Cahiez, Gerard; Knochel, Paul; Synlett; vol. 27; 3; (2016); p. 471 – 476;,
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. 25252-00-0, name is 2-Bromo-5-iodobenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C7H4BrIO2

Example I; 4-Bromo-3-hvdroxymethyl-1-iodo-benzene; Oxalyl chloride (13.0 mL) is added to an ice-cold solution of 2-bromo-5-iodo-benzoic acid in CH2CI2 (200 mL). DMF (0.2 mL) is added and the solution is stirred at room temperature for 6 h. Then, the solution is concentrated under reduced pressure and the residue is dissolved in THF (100 mL). The resulting solution is cooled in an ice-bath and LiBH4 (3.4 g) is added in portions. The cooling bath is removed and the mixture is stirred at room temperature for 1 h. The reaction mixture is diluted with THF and treated with 0.1 M hydrochloric acid. Then, the organic layer is separated and the aqueous layer is extracted with ethyl acetate. The combined organic layers are dried (Na2SO4) and the solvent is evaporated under reduced pressure to give the crude product. Yield: 47.O g (99% of theory)

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 25252-00-0.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; BOEHRINGER INGELHEIM PHARMA GMBH & CO. KG; WO2007/93610; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 5458-84-4, A common heterocyclic compound, 5458-84-4, name is 1-Iodo-2-methoxy-4-nitrobenzene, molecular formula is C7H6INO3, 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.

To a mixture of CuCN (322 mg, 3.6 mmol) and L-proline (415 mg, 3 mmol), in DMF (15 mL) under argon, 1-iodo-2-methoxy-4-nitrobenzene (837 mg, 3 mmol) was added at room temperature. The mixture was stirred at 80 C for 45 hours. The resulting suspension was cooled to room temperature, diluted with ethyl acetate (15 mL), and washed with water. The organic phase was dried over Na2SO4 and concentrated. The residue was purified by flash chromatography on silica with ethyl acetate-hexane to yield 2-methoxy-4-nitrobenzonitrile (463 mg, 87%).

The synthetic route of 5458-84-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NOVOGEN LIMITED; EIFFE, Eleanor; HEATON, Andrew; GUNNING, Peter; TREUTLEIN, Herbert; ZENG, Jun; JAMES, Ian; DIXON, Ian; (172 pag.)WO2016/187667; (2016); A1;,
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. 54435-09-5, name is 2-Iodo-4-methoxybenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 54435-09-5

(c) A mixture of 2-iodo-4-methoxybenzoic acid (13.6 g, 48.9 mmol), 5-amino-1-ethylpyrazole (5.5 g, 49 mmol), DMF (100 ml), K2 CO3 (6.9 g, 0.05 mol) and Cu(OAc)2 (0.5 g) is refluxed overnight. The reaction mixture is poured into water (500 ml) and acidified with acetic acid to a pH of 5-6. The product slowly crystallized from the solution and is collected by filtration and washed with water. The solid is taken up in CH2 Cl2 /methanol, dried, filtered and evaporated. The residue is combined with POCl3 (60 ml) and refluxed overnight. The reaction mixture is cooled, poured into water and neutralized with concentrated NH4 OH. The mixture is extracted with CH2 Cl2, and the CH2 Cl2 extracts are evaporated, and the residue is purified by column chromatography on silica gel eluding with ethyl acetate to afford 5 g of 1-ethyl-4-chloro-7-methoxy-1H-pyrazolo[3,4-b]quinoline, m.p. 114-115 C.

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 54435-09-5.

Reference:
Patent; Cell Pathways, Inc.; US5942520; (1999); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com