Category: iodides-buliding-blocks

Some common heterocyclic compound, 628-21-7, name is 1,4-Diiodobutane, molecular formula is C4H8I2, 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. Computed Properties of C4H8I2

General procedure: Under N2 atmosphere, LHMDS (1 M in THF, 3.0 equiv) was added to a cooled solution (0 C) of tricyclic lactam (1.0 equiv) dissolved in THF (6 mL). After stirring for 1 h at 0 C, an excess of alkyl halide (3.0 equiv for methyl iodide and 5.0 equiv for ethyl iodide) was added. For the introduction of five and six membered spirocyclic rings 1,4-diiodobutane or 1,5-diiodopentane (1.0 equiv) was added at 0 C. The solution was stirred for a further 3 h at 0 C. Completion of the conversion was confirmed by TLC. Saturated NaCl solution (10 mL) was then added and the mixture was extracted with EtOAc (3 × 10 mL). The organic layer was washed with NaCl solution (10 mL) and water (10 mL) and the aqueous layer was reextracted with EtOAc (2 × 10 mL). The combined organic layers were dried (Na2SO4), filtered, and the solvent was evaporated in vacuo and the residue was purified by FC.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 628-21-7, its application will become more common.

Reference:
Article; Sarkar, Soumya; Schepmann, Dirk; Wuensch, Bernhard; Tetrahedron Asymmetry; vol. 22; 13; (2011); p. 1411 – 1422;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 450412-28-9,Some common heterocyclic compound, 450412-28-9, name is 1-Bromo-3-chloro-2-iodobenzene, molecular formula is C6H3BrClI, 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 round bottom flask was charged with 13.45 g of phenylboronic acid, 110.29 mmol) was added dropwise a solution of 1-bromo-3-chloro-2-iodobenzene (35 g, 110.29 mmol), Pd (PPh3) 4 (1.27 g, 1.10 mmol), NaOH (4.41 g, 110.29 mmol), THF (485 mL) and water (243 mL). Then, the mixture is heated under reflux at 80 C . When the reaction is complete, dilute with distilled water at room temperature and extract with methylene chloride and water. The organic layer was dried over MgSO4 and concentrated. The resulting compound was purified by silicagel column and recrystallized to obtain 18.59 g of the product. (Yield: 63%)

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

Reference:
Patent; DUK SAN NEOLUX CO., LTD.; KIM, Hyo Jin; PARK, Nam Jin; KIM, Seul Gi; HWANG, Sun Pil; (46 pag.)KR2017/95602; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 328-73-4, 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. 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: In an open round-bottomed flask containing deionised water (20?25 mL), azido-alkyne (1, 1.0 equiv), aryl iodide (2, 2.0 equiv), cuprous oxide nanomaterials (15 mol percent), and Cs2CO3 (2.0 equiv) were added and stirred vigorously under sonication for 1?1.5 h at 80 °C, making sure that no halides escaped during the reaction. After that ethyl acetate was added in it and the mixture was centrifuged to separate the nanocatalyst. Aqueous phase was then again extracted with ethyl acetate repeatedly. Column chromatography afforded pure product (3a?k). The nanoparticles were washed with ethanol water(3) and dried under vacuum before reuse.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1-Iodo-3,5-bis(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Chatterjee, Nivedita; Pal, Rammyani; Sarkar, Swarbhanu; Sen, Asish Kumar; Tetrahedron Letters; vol. 56; 25; (2015); p. 3886 – 3889;,
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. 1829-28-3, name is Ethyl 2-iodobenzoate, A new synthetic method of this compound is introduced below., Safety of Ethyl 2-iodobenzoate

0.54 g (5 mmol) of 2.76 g (10 mmol) of o-phenylenediamine and ethyl iodobenzoate were weighed into a microwave reaction tube, and cuprous iodide (80 mg, 0.5 mmol), potassium phosphate (3.18 g, 15 mmol), Then, an appropriate amount of ethylene glycol and magnetron were added to the microwave reaction tube, and the microwave reaction was carried out under the protection of nitrogen at 180 C. After 1 h, the reaction was stopped, and the TLC detection was completed. Ethyl acetate (3 × 100 mL) and an appropriate amount of water and saturated NaCl solution were extracted, the organic layer was combined, an appropriate amount of anhydrous Na 2 SO 4 was added to remove water, suction filtration, and the filtered liquid was concentrated, and 1 g of silica gel was added for mixing.Separated using silica gel column chromatography,The eluent was (dichloromethane/methanol = 100/1) to give a bright yellow solid, 3, 0.68 g, yield 65%.

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; Xinxiang Medical University; Xinxiang Medical School San Quan College; Yan Fulin; Wang Yawen; Yan Jianwei; Yin Tiantian; Ma Jinshuo; (15 pag.)CN110183387; (2019); 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. 29289-13-2, name is 2-Iodo-4-methylaniline, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 29289-13-2

To a two-necked round-bottomed flask fitted with a guard tube, PBr3 (2.7mmol, 0.26 mL), DMF (3 mmol, 0.23 mL) and chloroform (0.80 mL) were added, allowed to cool to 0 C and stirred for 0.5 h. After formation of colourless solid complex, 2-Iodo-4-methyl-phenylamine 2b (1 mmol) in chloroform (5 mL) was added and the reaction mixture was allowed to stir at r.t. for another 1-2 h. After completion, the reaction mixture was neutralized by adding saturated NaHCO3 solution and then extracted with DCM (3X 20 mL). Combined organic layer was washed with brine and dried over Na2SO4. The solvent was evaporated under reduced pressure and the crude product was purified through column chromatography using silica gel (60-120 mesh) and petether/EtOAc (5:1) as eluent.

According to the analysis of related databases, 29289-13-2, the application of this compound in the production field has become more and more popular.

Reference:
Article; Ghosh, Munmun; Ahmed, Atiur; Singha, Raju; Ray, Jayanta K.; Tetrahedron Letters; vol. 56; 2; (2015); p. 353 – 355;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

19718-49-1, name is Methyl 4-amino-3-iodobenzoate, 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. name: Methyl 4-amino-3-iodobenzoate

To a stirred solution of Intermediate 14 (31.9 g, 107 mmol) in DMF (160 ml) was added methyl 4-amino-3-iodobenzoate (29.8 g 107 mmol), LiCl (4.5 g 107 mmol) and Na2CO3 (22.8 g 215 mmol). The resulting suspension was degassed, Pd(OAc)2 (0.96 g, 4.3 mmol) added, and degassing repeated. The reaction mixture was heated to HO0C for 50 minutes. The reaction mixture was then cooled to room temperature, filtered through celite and concentrated in vacuo. The resulting brown oil was separated between isopropyl acetate and water. The aqueous layer was back-extracted with isopropyl acetate (2 x 150 mL). The combined organic layers were dried (MgSO4), treated with decolourising charcoal (5% by weight of crude material) for 30 minutes at room temperature, and purified by column chromatography (SiO2, DCM) to give the title compound (9.0 g, 19%) as a pale cream solid. deltaeta (CDCl3) 8.50 (IH, br s), 8.05 (IH, s), 7.88 (IH, d), 7.32 (IH, d), 4.32 (IH, m), 3.99 (IH, t), 3.91 (3H, s), 3.65 (IH, d), 3.50-3.28 (3H, m), 3.05 (IH, dd), 1.48 (9H, s), 0.40 (9H, s). LCMS (ES+) 469.1 (M+Na).

The synthetic route of 19718-49-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; UCB PHARMA S.A.; WO2009/71888; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 19718-49-1, name is Methyl 4-amino-3-iodobenzoate, molecular formula is C8H8INO2, 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 4-amino-3-iodobenzoate

A solution of 3.00 g (10.8 mmol) of methyl 4-amino-3-iodobenzoate and 1.30 g (54.1 mmol) of lithium hydroxide in 150 ml of a dioxane/water mixture (1:1) was stirred at room temperature for 6 h. The dioxane was distilled off in vacuo, and the remaining aqueous phase was adjusted to pH 5 with 1 M hydrochloric acid. The precipitate was filtered off with suction and washed with water. 2.80 g (98%) of the title compound were obtained as a solid. HPLC (Kromasil RP-18, 60*2.1 mm, eluent=A: H2O+5 mL HClO4/L; B: acetonitrile; gradient=0-4.5 min 98% A-90% B; 4.5-6.5 min 90% B; 0.75 mL/min; temp.: 30 C., UV detection at 21 nm): Rt=3.51 min 1H-NMR (300 MHz in D6-DMSO) delta=5.98 (s, 2H), 6.74 (d, 1H), 7.63 (m, 1H), 8.10 (s, 1H), 12.33 (s, broad, 1H) MS (ESI+): m/z=281 [M+NH4]+

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 19718-49-1, its application will become more common.

Reference:
Patent; BAYER INTELLECTUAL PROPERTY GMBH; Hendrix, Martin; Boebeta, Frank-Gerhard; Erb, Christina; Krueger, Joachim; Luithle, Joachim; Methfessel, Christoph; Schreiber, Rudy; Wiese, Welf-Burkhard; US9139579; (2015); B2;,
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. 624-75-9, name is 2-Iodoacetonitrile belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Formula: C2H2IN

To a mixture of 5-bromo-2-isopropyl-4-methoxy-phenol from step 4 (0.831 g, 3.4 mmol) and K2CO3 (0.562 g, 4.1 mmol) in 17 mL dimethyl formamide (DMF) was added iodoacetonitrile (0.594 g, 3.6 mmol). The mixture was warmed to 60 C. for 30 minutes and then allowed to cool to room temperature. After cooling to room temperature the mixture was taken up in 50 mL of H2O and extracted with 1:1 toluene/ethyl acetate, washed with H2O and then with brine. The combined organic layers were dried over Na2SO4, filtered and conectrated in vacuo to give a crude solid. Purification via flash chromatography (1:1 hexane/CH2Cl2) afforded (5-bromo-2-isopropyl-4-methoxy-phenoxy)-acetonitrile (0.611 g, 63%) as a while solid.

The synthetic route of 624-75-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Roche Palo Alto LLC; US2005/209260; (2005); 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. 645-00-1, name is 1-Iodo-3-nitrobenzene, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 645-00-1

General procedure: A mixture of the aryl halide (0.5 mmol), phenylacetylene(0.5 mmol), piperidine (1 mmol), ortho-palladated catalyst(0.2 mol %) was added to NMP (3 mL) in round-bottom flask equipped with condenser and placed into the Milestone microwave. Initially using a microwave power of 600 W the temperature was ramped from room temperature to 100 C and then held at this temperature until the reaction was completed. During this time, the power was modulated automatically to keep the reaction mixture at 100 C. The mixture was stirred continuously during the reaction and monitored by both TLC and GC. After the reaction was complete, the mixture was cooled to room temperature and was diluted with n-hexane and water. The organic phase was dried over MgSO4, filtered and concentrated under reduced pressure using rotary evaporator. The residue was purified by silica gel column chromatography.

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 645-00-1.

Reference:
Article; Hajipour, Abdol R.; Rafiee, Fatemeh; Journal of the Iranian Chemical Society; vol. 12; 7; (2015); p. 1163 – 1169;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 69113-59-3, These common heterocyclic compound, 69113-59-3, name is 3-Iodobenzonitrile, 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.

The title compound (40 mg, 66.4 %, white solid) was obtained from [4- [1- (5-] [TRIBUTYLSTANNANYL-ISOXAZOL-3-YL)-ETHYL]-PIPERAZINE-1-CARBOXYLIC] acid ethyl ester (109 mg, 0.2 mmol) and Pd (PPh3) [2C12] (2.0 mg) with 3-iodo-benzonitrile (45.7 mg, 0.17 mmol) in dioxane [(LUT)] at [110 C OVERNIGHT. LH-NMR (CDCL3) B] (ppm): [8.] 07 (s, 1H), 8.05 (d, 1H), 7.63 (d, 1H), 7.62 (t, [1H),] 6.62 (s, [1H),] 4.12 (q, 2H), 3.88 (q, [1H),] 3.50 (m, 4H), 2.52 (m, 4H), 1.47 (d, 3H) and 1.25 (t, 3H).

Statistics shows that 3-Iodobenzonitrile is playing an increasingly important role. we look forward to future research findings about 69113-59-3.

Reference:
Patent; ASTRAZENECA AB; NPS PHARMACEUTICALS, INC.; WO2004/14370; (2004); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com