Month: March 2021

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. 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of Methyl 5-bromo-2-iodobenzoate

500ml three-necked round bottom flask was charged with methyl 5-bromo-2-iodo benzoate (130g, 0.381mol), as 9-phenanthrene boronic acid(84.7g, 0.381mol), 2% of tetrakis triphenylphosphine palladium (8.82g, 0.008mol), 2M potassium carbonate (100ml), tetrahydrofuran (200ml) was added. 16 hours with stirring and reflux under reduced pressure and then extracted with ethyl acetate concentrate was purified by silica gel column (ethyl acetate: heptane = 1: 5) to give the [intermediate 1-a] (120g, yield = 80.4%).

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 181765-86-6.

Reference:
Patent; SFC CO., LTD.; JU MAN, SONG; HEE DAE, KIM; YUR IM, LEE; SANG WOO, PARK; PARK, SEOK BAE, PARK; KYUNG SEOK, JEONG; SOON WOOK, CHA; (36 pag.)KR2015/113642; (2015); A;,
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. 6326-42-7, name is Methyl 2-iodo-4-nitrobenzoate, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C8H6INO4

To a mixture of ammonium chloride (122 g) and iron (38.2 g) in ethanol (1000 mL) and water (100 mL) was added Example 2.140.2 (70 g,) at room temperature. The mixture was stirred at 80 C for 4 hours and filtered to remove insoluble material. The filtrate was concentrated under reduced pressure. The residue was dissolved in ethyl acetate (1000 mL) and washed with water (500 mL). The aqueous phase was extracted with ethyl acetate (1000 mL x 2). The combined organic phase was washed with brine, dried over MgSO4, filtered and concentrated to give the title compound. MS (LC-MS) m/e 278.0 (M+H)+.

According to the analysis of related databases, 6326-42-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ABBVIE INC.; BENATUIL, Lorenzo; BRUNCKO, Milan; JUDD, Andrew, S.; LI, Yingchun; MCCLUSKEY, Andrew; PHILLIPS, Andrew, C.; PHILLIPS, Darren, C.; SEAGAL, Jane; SOUERS, Andrew, J.; (808 pag.)WO2017/214462; (2017); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 6940-76-7, name is 1-Chloro-3-iodopropane, molecular formula is C3H6ClI, 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. SDS of cas: 6940-76-7

a) Freshly prepared LDA (8.97 mmol) was added to a solution of 2-fluoro-3- iodopyridine (2.00 g, 8.97 mmol) in THF (15 mL) cooled at -78 C. After 1 h, 1 – chloro-3-iodopropane (0.96 mL, 8.97 mmol) was added to the anion solution, allowing to reach room temperature (overnight). The reaction volume was reduced to ca. 10 mL and the mixture was poured over EtAcO (60 mL) and washed with water (2 x 20 mL); the organic layer was dried over anhydrous Na2S04 and filtered. After removal of the solvent, the residue was purified by column chromatography on silica gel (2>4% EtAcO/hexanes), affording 1 .88 g of 3-(3-chloropropyl)-2-fluoro-4- iodopyridine [Rf= 0.70 (5% EtAcO/hexanes), colorless oil, 70% yield].LC-MS ESI+ m/z: 300 (M+1 , 98%) (Method 5).1 H-NMR (CDCI3, 250 MHz, ?): 7.70 (d, J= 5.2 Hz, 1 H, ArH); 7.61 (d, J= 5.2 Hz, 1 H, ArH); 3.62 (t, J= 6.5 Hz, 2H); 2.99-2.90 (m, 2H); 2.10-1 .97 (m, 2H

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 6940-76-7, its application will become more common.

Reference:
Patent; LABORATORIOS DEL DR. ESTEVE, S.A.; DRACONIS PHARMA, S.L.; ALMIRALL, S.A.; TORRENS JOVER, Andoni; MERCE VIDAL, Ramon; CALDENTEY FRONTERA, Francesc Xavier; RODRIGUEZ GARRIDO, Antonio, David; CARCELLER GONZALEZ, Elena; SALAS SOLANA, Jordi; WO2013/37960; (2013); A1;,
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. 123158-75-8, name is 4-Chloro-2-iodo-6-nitroaniline, A new synthetic method of this compound is introduced below., name: 4-Chloro-2-iodo-6-nitroaniline

Example B4 Preparation of 4-chloro-6-iodo-1.2-phenylenediamine 1.5 g of 4-chloro-2-iodo-6-nitroaniline together with 50 ml of tetrahydrofuran and 10 ml of 1-propanol are initially introduced into a stirred autoclave. 5 mg of FeCl2.4H2 O and 0.3 g Pt/Pb-CaCO3 catalyst are added to the solution, and hydrogenation is carried out at 130 C. and 20 bar of hydrogen. After the hydrogenation has come to a standstill, the reaction mixture is cooled to room temperature, the reactor is rendered inert with nitrogen and the catalyst is filtered off. After filtration, the solvent is removed by distillation to give 1.3 g of 4-chloro-6-iodo-1,2-phenylenediamine as a crude product. 1 H-NMR (CDCI3, 300MHz) 3.56 ppm (s, 2H, broad); 3.77 ppm (s, 2H, broad); 6.68 ppm (s, 1H); 7.18 ppm (s, 1H).

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; Novartis Consumer Health S.A.; US5877340; (1999); 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. 4949-69-3, name is 4-Iodo-3-methylaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: iodides-buliding-blocks

EXAMPLE 271A 2-bromo-N-(4-iodo-3-methylphenyl)acetamide The procedure described in Example 1A was followed, substituting 4-iodo-3-methylaniline for 3-methylaniline to provide the title compound as a white solid. 1H NMR (300 MHz, DMSO-d6) delta 2.33 (s, 3H), 4.02 (s, 2H), 7.20 (dd, 1H, J=8.5, 2.4 Hz), 7.56 (d, 1H, J=2.4 Hz), 7.74 (d, 1H, J=8.5 Hz), 10.40 (br s, 1H); MS (DCI/NH3) m/e 353/355 (M+H)+; 371.373 (M+NH4)+.

The synthetic route of 4949-69-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bhatia, Pramila A.; Daanen, Jerome F.; Hakeem, Ahmed A.; Kolasa, Teodozyj; Matulenko, Mark A.; Mortell, Kathleen H.; Patel, Meena V.; Stewart, Andrew O.; Wang, Xueqing; Xia, Zhiren; Zhang, Henry Q.; US2004/29887; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

52548-14-8, name is 2-Iodo-5-methylbenzoic acid, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. COA of Formula: C8H7IO2

Step 1) Synthesis of 5-methyl-2- (2H-1, 2, 3-triazol-2-yl) benzoic acid To a solution of N, N-dimethylformamide (30 mL) were added sequentially 2H-1, 2, 3-triazole (3.45 g, 50 mmol) , 2-iodo-5-methyl benzoic acid (5.24 g, 20 mmol) , cesium carbonate (11.72 g, 36 mmol) , trans-N, N’-dimethyl-1, 2-cyclohexanediamine (0.51 g, 3.6 mmol) and cuprous iodide (0.38 g, 2 mmol) . The reaction was heated to 100 ? under N2. After reaction for 4 hours, the reaction mixture was cooled to rt, diluted with water (60 mL) and extracted with ethyl acetate (200 mL ¡Á 2) . The aqueous layer was acidified to pH 1 to 2 with concentrated hydrochloric acid, and then extracted with ethyl acetate (200 mL ¡Á 2) . The combined organic layers were dried over anhydrous sodium sulfate, and filtered. The filtrate was concentrated in vacuo and the residue was purified by silica gel column chromatography (DCM/methanol (v/v) =50/1) to give the title compound as a yellow solid (2.76 g, 68 %) .MS (ESI, neg. ion) m/z: 202.1 [M-H] -;1H NMR (CD3OD, 600 MHz) d (ppm) : 7.88 (s, 2H) , 7.66 (d, 1H) , 7.59 (d, J= 8.2 Hz, 1H) , 7.50-7.48 (dd, J = 8.1 Hz, 1.1 Hz, 1H) , 2.45 (s, 3H) ; and13C NMR (CD3OD, 151 MHz) d (ppm) : 169.8, 140.7, 137.5, 136.7, 133.5, 131.5, 129.3, 126.0, 21.0.

The synthetic route of 52548-14-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SUNSHINE LAKE PHARMA CO., LTD.; ZHANG, Yingjun; JIN, Chuanfei; ZHANG, Ji; (90 pag.)WO2017/88759; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 18698-96-9, A common heterocyclic compound, 18698-96-9, name is 2-(2-Iodophenyl)acetic acid, molecular formula is C8H7IO2, 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-(2-Iodophenyl)acetic acid (100 g, 381.67 mmol) was dissolved in MeOH (400 mL). SOC12 (34 mL, 458.01 mmol) was added at RT with stifling, and the reaction mixture was heated at 60 C for 1 h. The solvent was removed in vacuo. The resulting crude material was dissolved in ethyl acetate (250 mL), washed with saturated NaHCO3 (1 x 100 mL), brine (1 x 100 mL) and dried (Na2SO4). The solvent was removed to afford methyl 2-(2- iodophenyl)acetate (100 g, 95%) as a brown oil. MS (ESI) mlz 276.9 [M+H].

The synthetic route of 18698-96-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ZENO ROYALTIES & MILESTONES, LLC; HUANG, Peter, Qinhua; BOREN, Brant, Clayton; BUNKER, Kevin, Duane; LIU, Hui; PALIWAL, Sunil; (99 pag.)WO2019/28008; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 108078-14-4, 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 108078-14-4 as follows.

General procedure: To a solution of p-tolylhydrazine hydrochloride (0.79 g, 5 mmol), 2-chlorobenzoic acid (0.78 g, 5 mmol), and HCTU (2.28 g, 5.5 mmol) in DMF (10.0 mL), Et3N (2.08 mL, 15 mmol) was added. The mixture was stirred at r.t. overnight. Then the mixture was washed with sat. aq NH4Cl, aq NaHCO3, and brine. The organic layer was dried (MgSO4) and the solvent was removed under reduced pressure. The residue was purified by column chromatography (petroleum ether/EtOAc,5:1) to give 1b (0.78 g, 60%) as a white solid; mp 161.3-162.4 C.

According to the analysis of related databases, 108078-14-4, the application of this compound in the production field has become more and more popular.

Reference:
Article; Wang, Wei-Juan; Chen, Jia-Hua; Chen, Zi-Cong; Zeng, Yu-Feng; Zhang, Xue-Jing; Yan, Ming; Chan, Albert S. C.; Synthesis; vol. 48; 20; (2016); p. 3551 – 3558;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 63262-06-6, A common heterocyclic compound, 63262-06-6, name is 1,4-Dibromo-2,5-diiodobenzene, molecular formula is C6H2Br2I2, 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.

A nitrogen gas atmosphere was prepared in a reaction vessel equipped with a stirrer, then, a compound 1 (22.0 g), 2-bromophenylboronic acid (19.1 g), tetrakis(triphenylphosphine)palladium(0) (2.43 g) and tetrahydrofuran (440 mL) were added, and the mixture was heated at 45 C. Thereafier, to this was added silver carbonate (47.2 g), and the mixture was refluxed for 3 hours. The resultant reaction liquid was cooled down to room temperature, then, water and toluene were added, and the mixture was stirred at room temperature. Thereafter, the aqueous layer was separated, and the organic layer was washed with a saturated sodium chloride aqueous solution. To the resultant organic layer was added sodium sulfate, then, the layer was filtrated, and concentrated to obtain a coarse product. Thereafier, to this were added toluene and activated carbon, and the mixture was stirred at 70 C. for 1 hour. Thereafter, the mixture was filtrated through a filter pre-coated with Celite. The resultant residue was washed with toluene several times. The resultant washing liquid was concentrated, then, recrystallized using toluene, thereby obtaining 17.9 g of a compound 2 (yield:74%, purity: 98.9%) as a white solid. ?H-NMR (DMSO-d5, 300 MHz): oe (ppm)7.43 (4H, t), 7.49 (2H, t), 7.71 (2H, d), 7.76 (2H, d).

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; Sumitomo Chemical Company, Limited; USUI, Motoaki; FUKUSHIMA, Daisuke; TANAKA, Shin-ya; (58 pag.)US2017/137566; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 766-85-8,Some common heterocyclic compound, 766-85-8, name is 3-iodoanisole, molecular formula is C7H7IO, 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.

i) l-Bromo-2-iodo-4-methoxy-benzene Bromine (2.8 mL, 54.49 mmol) was added dropwise over 5 minutes to a solution of 3- iodoanisole (10.01 g, 42.77 mmol) in glacial acetic acid (65 mL). The resulting orange solution was stirred at room temperature for 24 hours. The reaction mixture was diluted with water and extracted with hexane. The combined extracts were washed with aqueous sodium thiosulfate solution (5%) and brine, dried over magnesium sulfate and concentrated under reduced pressure to give 13.51 g (quantitative yield) of the title compound. 1H NMR (400 MHz, CDCl3) delta ppm 7.47 (d, 1 H) 7.39 (d, 1 H) 6.77 (dd, 1 H) 3.77 (s, 3 H).

The synthetic route of 766-85-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTRAZENECA AB; BYLUND, Johan; EK, Maria, E; HOLENZ, Joerg; KERS, Annika; OeHBERG, Liselotte; WO2010/132016; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com