Month: January 2021

Application of 627-31-6, The chemical industry reduces the impact on the environment during synthesis 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), I believe this compound will play a more active role in future production and life.

LiHMDS (56.2 mL, 56 mmol, 1 M solution in THF) was added drop wise to a stirred yellow solution of methyl 2-(pyrimidin-5-yl)acetate (8.00 g, 47 mmol) in THF (150 mL) at -70 C under N2 and the reaction was stirred at -70 C for 1 hr. A solution of 1 ,3-diiodopropane (13.8 g, 46.8 mmol) in THF (20 mL) was added drop wise to the reaction at -70 C and the mixture allowed to warm to 20 C slowly and stirred for 1 hr. The reaction mixture was again cooled to -70 C and an additional portion of LiHMDS (1 M in THF, 56.2 mL, 56.2 mmol) was added drop wise. After addition, the reaction was allowed to warm to 20 C slowly and stirred for an additional hour. The reaction was poured into saturated NH4CI solution (60 mL) the mixture extracted with EtOAc (300 mL x 3). The combined organic extracts were washed with brine, dried (Na2S04) filtered and concentrated in vacuo. The crude product was purified by column chromatography on silica gel eluting with pet. ether: EtOAc (100:0 to 65:35) to afford the title compound as a yellow oil, 1 .95 g, 22% yield. 1H NMR (400 MHz, CDCI3): 1 .90-2.04 (m, 1 H), 2.12- 2.25 (m, 1 H), 2.48-2.59 (m, 2H), 2.87-2.96 (m, 2H), 3.67 (s, 3H), 8.66 (s, 2H), 9.09 (s, 1 H). LCMS m/z = 193 [M+H]+

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, 1,3-Diiodopropane(stabilized with Copper chip), other downstream synthetic routes, hurry up and to see.

Reference:
Patent; PFIZER INC.; CASIMIRO-GARCIA, Agustin; STROHBACH, Joseph Walter; HEPWORTH, David; LOVERING, Frank Eldridge; CHOI, Chulho; ALLAIS, Christophe Philippe; WRIGHT, Stephen Wayne; (213 pag.)WO2018/11681; (2018); 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. 620621-48-9, name is Methyl 2-chloro-5-iodobenzoate, A new synthetic method of this compound is introduced below., SDS of cas: 620621-48-9

106.1 Sodium 2-chloro-5-(pyridin-4-yloxy)benzoate A microwave vial was charged with copper (I) bromide (23 mg), Cs2CO3 (2055 mg), 4-hydroxypyridine (300 mg) and methyl-2-chloro-5-iodobenzoate (1122 mg) and flushed with argon. DMSO (4.7 mL) was added followed by 2-pyridyl acetone (0.043 mL) and the reaction mixture was heated to 100 C. for 3 h in the microwave. It was diluted with EtOAc, filtered and the filtrate was washed with H2O. The aqueous phase was basified with a 1M solution of NaOH and extracted with EtOAc. The crude was purified by CC(RP C18, H2O/CH3CN 1/0 to 8/2) to give 1.2 g of the titled compound as a white powder. LC-MS (B): tR=0.34 min; [M+H]+: 249.98

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; Actelion Pharmaceuticals Ltd.; Hilpert, Kurt; Hubler, Francis; Murphy, Mark; Renneberg, Dorte; US2014/73651; (2014); 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. 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene, A new synthetic method of this compound is introduced below., Product Details of 401-81-0

The N-nucleophile (2.21 mmol), Cu2O (Sigma-Aldrich, 99.99% purity, 0.147-0.294 mmol), K3PO4(2.94 mmol), the aryl halide (1.47 mmol), phase transfer catalyst (0.147-0.294 mmol) and water(0.40 mL) were added to a reaction vial and a screw cap was fitted to it. The reaction mixture wasstirred under air in a closed system at 130C for 24 h, then the heterogeneous mixture was cooledto RT and diluted with dichloromethane. The resulting solution was directly filtered through apad of Celite. The combined organic extracts were dried with anhydrous Na2SO4 and the solventwas removed under reduced pressure. The crude product was purified by silica-gel columnchromatography to afford the N-arylated product. The identity and purity of all products wasconfirmed by 1H and 13C NMR spectroscopic analysis.

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; Yong, Fui-Fong; Teo, Yong-Chua; Chua, Guan-Leong; Lim, Gina Shiyun; Lin, Yizhen; Tetrahedron Letters; vol. 52; 11; (2011); p. 1169 – 1172;,
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. 51560-21-5, name is 1,4-Diiodo-2,5-dimethoxybenzene, A new synthetic method of this compound is introduced below., Application In Synthesis of 1,4-Diiodo-2,5-dimethoxybenzene

A two-neck round bottom flask (250ml) was cooled to -63 C in a liquid nitrogen/chloroform slush bath to which 1,4-diiodo 2,5-dimethoxybenzene (2.0g, 5.1mmol, 1.0 equiv) was dissolved in dichloromethane (40ml) under nitrogen. BBr3 (12ml, 1.0M, 12mmol) was then added dropwise through a septa seal using a syringe. The mixture was allowed to warm to room temperature and stirred for 24hrs and then carefully quenched with water (75ml). The aqueous layer was then extracted with ether (3 * 50ml). The combined organic phases were extracted with NaOH (150ml, 2N). The NaOH solution was then neutralized in dilute HCl in an ice bath to form a pink precipitate that was collected and dried. The resultant solid material was recrystallized from toluene to give light brown crystals, (1.48g, 80%).

The synthetic route of 51560-21-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Tsakama, Madalitso; Shang, Yuting; He, Yonghuang; Fan, Bei; Wang, Fengzhong; Chen, Weihua; Dai, Xiaofeng; Tetrahedron Letters; vol. 57; 16; (2016); p. 1739 – 1742;,
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. 54507-44-7, name is 2-Iodo-4-(trifluoromethyl)benzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 2-Iodo-4-(trifluoromethyl)benzoic acid

4) Synthesis of 2-[(3-chloro-4-methoxyphenyl)thio]-4-(trifluoromethyl)benzoic acid (compound 211-4) [0358] N,N-dimethylformamide (90 ml) was added copper powder (360 mg), and the mixture was stirred at 120C for 3 hr. The reaction mixture was cooled, 1M hydrochloric acid and ethyl acetate were added, an insoluble material was filtered off, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography and the obtained solid was washed with hexane to give compound 211-4 (12.6 g) as a white solid. 1H-NMR(DMSO-d6)delta(ppm):3.95(3H,s), 6.90(1H,s), 7.33(1H,d,J=8.6Hz), 7.55-7.61(2H,m), 7.71(1H,d,J=2.4Hz), 8.12(1H,d,J=8.6Hz), 13.8(1H,brs).

The synthetic route of 54507-44-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Mitsubishi Tanabe Pharma Corporation; HAMADA, Maiko; TASHIRO, Kaoru; SAKASHITA, Hiroshi; KIUCHI, Masatoshi; TAKEDA, Shuzo; ADACHI, Kunitomo; EP2842937; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 88-67-5, 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 88-67-5 as follows.

Prepared according to literature procedure. A solution of 2-iodobenzoic acid (1,240 mg, 5.0 mmol) in Conc. H2SO4 ( 10.00 mL) was heated at 60 C for 20 minutes. The solution was yellow orange. Then N-bromosuccinimide (1,668 mg, 6.0 mmol) was added in three portions each during 15 minutes. The mixture was brown and allowed to stir for 2 hours. After the reaction was completed, filtered and wash with cold water. A white solid was obtain. The aqueous eluted was extracted with EtOAc, the organic extracts were washed with brine, dried over anhydrous Na2SO4, filtered and concentrated that to obtain white solid. 1H NMR (300 MHz, CDCl3) delta 8.12 (d, J = 2.4 Hz, 1H), 7.90 (d, J = 8.4 Hz, 1H), 7.33 (dd, J = 8.4, 2.4 Hz, 1H); 13C NMR (75 MHz, CDCl3) delta 169.7, 143.2, 136.6, 134.9, 134.7, 122.4, 92.7. Other data was identical to the literature values.

According to the analysis of related databases, 88-67-5, the application of this compound in the production field has become more and more popular.

Reference:
Article; Duangjan, Chanikan; Rukachaisirikul, Vatcharin; Saithong, Saowanit; Kaeobamrung, Juthanat; Tetrahedron Letters; vol. 59; 39; (2018); p. 3537 – 3540;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 89459-38-1,Some common heterocyclic compound, 89459-38-1, name is 2-Iodo-4-nitrobenzoic acid, molecular formula is C7H4INO4, 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 mixture of Example 2.140.1 (130 g) in a mixture of methanol (1000 mL) and sulfuric acid (23.65 mL) was stirred at 85 C. for 16 hours and concentrated to dryness. The residue was triturated with methanol (100 mL) and the suspension was stirred for 10 minutes. The solid was collected by filtration, washed with water (200 mL*3) and methanol (20 mL), and air-dried for 16 hours to give the title compound. MS (LC-MS) m/e 308.0 (M+H)+.

The synthetic route of 89459-38-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AbbVie Inc.; Benatuil, Lorenzo; Bruncko, Milan; Chao, Debra; Izeradjene, Kamel; Judd, Andrew S.; Phillips, Andrew C.; Souers, Andrew J.; Thakur, Archana; (556 pag.)US2017/355769; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 7681-82-5, name is Sodium iodide, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 7681-82-5, Computed Properties of INa

To a dry round-bottom flask with a stir bar was added 5c (245 mg, 0.983 mmol) and NaI (460 mg, 3.06 mmol). Chlorotrimethylsilane (375 muL, 2.95 mmol) was added dropwise over 5 min at 0C, allowed to stir at 0C for 5 more min, and warmed to rt for 3 hr. The mixture was concentrated, dissolved in ether (25 mL) and 1M HCl (~10 mL), and transferred to a separatory funnel. The aqueous layer was extracted once more with ether (25 mL) and combined organics were washed once with with sat?d NaHSO3 and once with sat?d brine. The organic layer was dried over Na2SO4, filtered, concentrated, and dried in vacuo to afford a dry, white solid 7 (181 mg, 72%) which did not require further purification .1H NMR (CDCl3, 400 MHz) delta 4.52 (s, 2H), 5.06 (s, 2H), 7.29 (d, 1H, J=7.9), 7.51 (d, 1H, J=7.8), 7.75 (s, 1H).13C NMR (CDCl3, 100 MHz) delta 5.47, 71.21, 121.66, 130.50, 131.77, 138.51, 153.53. 11B NMR (CDCl3, 128 MHz) delta 32.24. HRMS (MAII) calc. for C8H8BO2 [M-I]+ 147.0612, found 147.0623.

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, Sodium iodide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; UNIVERSITY OF THE SCIENCES; TOMSHO, John, W.; GAMRAT, James, M.; (0 pag.)WO2019/173814; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 191348-14-8, These common heterocyclic compound, 191348-14-8, name is 2-Iodo-4-methoxyaniline, 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 solution of 2-iodo-4-methoxyaniline 30-d ( 1.00 g, 4.02 mmol) in DMF cooled to 0C were sequentially added diethylamine (419 uL, 4.02 mmol), copper(I) iodide (143 mg, 0.80 mmol) and dichlorobis(triphenylphosphine) palladium (II) (282 mg, 0.40 mmol). After complete dissolution of copper(I)iodide, propyl 3,3-dimethylhex-5-ynoate 1 1-d (805 mg, 4.42 mmol) was added dropwise at 0C and the reaction was then stirred at room temperature overnight. Water and ethyl acetate were added; the organic layer was separated, washed with saturated aqueous ammonium chloride and brine, dried over anhydrous MgS04, filtered and concentrated in vacuo. Purification by silica gel chromatography provided intermediate 30-e as a beige oil. MS (m/z) M+H=304

The synthetic route of 191348-14-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PHARMASCIENCE INC.; BUREAU, Patrick; FOURNIER, Jean-Hugues; JAQUITH, James B.; LAURENT, Alain; ROSE, Yannick; PROULX, Melanie; MORRIS, Stephen; WO2012/126084; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 1000801-26-2, These common heterocyclic compound, 1000801-26-2, name is 4-(Difluoromethoxy)-2-iodoaniline, 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.

INTERMEDIATE 7 (METHOD H)fert-Butyl (35)-3-[3-(trimethylsilv?prop-2-vn- 1 -yllmophiholine-4-carboxylateTo a solution of Intermediate 6 (8.05 g, 35.7 mmol) dissolved in anhydrous THF (250 mL) at 00C was added n-butyllithium (15.7 mL, 39.3 mmol, 2.5 M in hexanes) dropwise over 15 minutes. After stirring for 30 minutes, chlorotrimethylsilane was added slowly over 5 minutes and the reaction mixture stirred for 45 minutes and then allowed to warm to r.t. After stirring at r.t. for 18 h, the reaction mixture was quenched by the addition of water (ca 1 mL) and the solvent was removed in vacuo. The crude mixture was dissolved in DCM and washed with water, the aqueous phase was extracted with further DCM (500 mL) and the combined organic fractions were dried using an Isolute phase separator cartridge and concentrated in vacuo to give a dark brown oil. Purification by column chromatography (SiO2, 5-20% EtOAc/hexanes) gave the title compound (8.1 g, 76%) as a colourless oil and recovered starting material (1.25 g, 15%). delta? (CD3OD) 3.91 (IH, m), 3.82 (IH, d, J 11.7 Hz), 3.70 (IH, dd, J 3.6 and J 11.4 Hz), 3.58 (IH, dd, J 2.9 and J 13.7 Hz), 3.40-3.20 (2H, m), 2.95 (IH, m), 2.60 (IH, dd, J9.1 and J 16.7 Hz), 2.38 (IH, dd, J6.4 and J 16.7 Hz), 1.35 (9H, s), 0.00 (9H, s).

The synthetic route of 1000801-26-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; UCB PHARMA S.A.; WO2009/1089; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com