Tag: M.W=300-400

Synthetic Route of 51839-15-7, These common heterocyclic compound, 51839-15-7, name is Dimethyl 5-iodoisophthalate, 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.

Dimethyl-5-iodoisophthalate (1.35 g, 4.21 mmol, Matrix Scientific, Columbia, SC) and lithium hydroxide monohydrate (884 mg, 20.07 mmol) were taken in a mixture of 3.95 mL methanol and 0.99 mL water and the suspension was stirred vigorously at 20 C for 3.5 h. The mixture was diluted with aqueous saturated sodium bicarbonate to a volume of 75 mL, and unreacted ester was removed by extraction with 75 mL ethyl acetate. The aqueous layer was carefully acidified with 1 M HCl to pH 2 and the resultant acid was extracted twice with 250 mL ethyl acetate. The ethyl acetate fractions were combined, dried over sodium sulfate, and the ethyl acetate was evaporated to give a white powder (965 mg, 78.4%): mp 302-303 C 1H NMR-300 MHz (CD3OD) delta 8.55 (d, 2H), 8.60 (d, 1H). 13C NMR (126 MHz, CD3OD) delta 92.6, 129.5, 132.6, 142.2, 165.7. MS (LCMS-ESI; negative ion mode) m/z: 290.7 (M-H)-; HRMS (FAB-) Calcd for C8H4IO4 (M-H)- 290.9154. Found 290.9141 ¡À 0.0000 (n = 2).

The synthetic route of 51839-15-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Vaidyanathan; White; Affleck; Zhao; Welsh; McDougald; Choi; Zalutsky; Bioorganic and Medicinal Chemistry; vol. 20; 24; (2012); p. 6929 – 6939;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 181765-86-6, These common heterocyclic compound, 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, 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.

In a 500-mL round-bottom flask reactor, methyl 5-bromo-2-iodobenzoate (25.0 g, 73 mmol), 4-dibenzofuran boronic acid (18.7 g, 88 mmol), tetrakis (triphenylphosphine)palladium (1.7 g, 0.15 mmol), and potassium carbonate (20.2 g, 146.7 mmol) were stirred together with toluene (125 mL), tetrahydrofuran (125 mL), and water (50 mL) for 10 hrs at 80 C. After completion of the reaction, the reaction mixture was cooled to room temperature and extracted with ethyl acetate. The organic layer thus formed was separated, concentrated in a vacuum, and purified by column chromatography to afford (75.0 g, 60.1%).

Statistics shows that Methyl 5-bromo-2-iodobenzoate is playing an increasingly important role. we look forward to future research findings about 181765-86-6.

Reference:
Patent; SFC CO., LTD.; LEE, Chang-Hee; SEO, Hyun-JONG; YOON, Seo-Yeon; SHIM, So Young; KIM, Si-In; (214 pag.)US2018/233669; (2018); 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. 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone, This compound has unique chemical properties. The synthetic route is as follows., name: 2-Bromo-1-(4-iodophenyl)ethanone

General procedure: The appropriate carbonyl compound (50 mmol) was dissolved in 50 mL of ethanol and magnetically stirred with an equimolar quantity of thiosemicarbazide for 24 h at room temperature with catalytic amounts of acetic acid. The desired thiosemicarbazone precipitated from reaction mixture, was filtered, crystallized from suitable solvent, and dried. Equimolar quantities of 4-iodo-acetophenone and bromine, both dissolved in chloroform, were stirred for 4 h at room temperature until the presence of HBr disappeared. The solution was evaporated under vacuum and the obtained pale yellow solid was washed with petroleum ether to give alpha-bromo-4-iodo-acetophenone in good yield (94%). Equimolar amounts of the prepared thiosemicarbazone (50 mmol) and alpha-bromo-4-iodo-acetophenone (50 mmol), both suspended in 50 mL of ethanol, were reacted at room temperature under magnetic stirring for 10 h. The precipitate was filtered and purified by chromatography to give compounds 1-25 in high yield.

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 31827-94-8.

Reference:
Article; Secci, Daniela; Bizzarri, Bruna; Bolasco, Adriana; Carradori, Simone; D’Ascenzio, Melissa; Rivanera, Daniela; Mari, Emanuela; Polletta, Lucia; Zicari, Alessandra; European Journal of Medicinal Chemistry; vol. 53; (2012); p. 246 – 253;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene, 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 328-73-4, name: 1-Iodo-3,5-bis(trifluoromethyl)benzene

EXAMPLE 7 Preparation of 2-(3,5-bis-(trifluoromethyl)-phenyl)-indene 20 ml of triethylamine, 2.2 g (20 mmole) of indene, 6.8 g (20 mmole) of 1-iodo-3,5-bis(trifluoromethyl)-benzene and 0.134 g (0.6 mmole) and 0.134 g (0.6 mmole) of Pd(OAc)2 were stirred under relux for 12 h. After it all triethylamine was removed under reduced pressure. The residue was treated with the mixture 50 ml of water and 50 ml of diethyl ether. Etherial layer was separated, washed twice with water, filtered and dried over Na2SO4. Ether was removed and some 20 ml of pentane were added to the reaction mixture, it was cooled down to -20¡ã C. and product was crystallized as dark needle crystals, which were filtered, washed with small portion of cold pentane and dried in vacuum. The yield of product was 32percent. 1H NMR (CDCl3): 8.06 (bs, 2H); 7.80 (bs, 1H); 7.58-7.48 (m, 3H); 7.42-7.32 (m, 2H); 3.88 (s, 2H).

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:
Patent; Montell Technology Company bv; US6271411; (2001); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 915095-86-2, name is (2-Chloro-5-iodophenyl)(4-fluorophenyl)methanone, molecular formula is C13H7ClFIO, 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 (2-Chloro-5-iodophenyl)(4-fluorophenyl)methanone

(5-iodo-2-chlorophenyl) (4-fluorophenyl) methanone (18.03 g, 50 mmol) was added DMS0 (80 mL) Ice bath slowly add lithium ethoxide (3.128,1.2 called), After adding 0 ¡ã (below the stirring reaction 311, hole (after the reaction is completed, add water (240mL) slowly under ice bath, Stirring crystallization lh, Filter, The filter cake was washed with water (200 mL) Beat with ethanol (50 mL) Filter, Dried to give 15.99 g of a pale yellow solid of compound lib, yield: 82.7percent, purity: 99.44percent.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 915095-86-2, its application will become more common.

Reference:
Patent; Shanghai Pharmaceutical Industry Institute; China Pharmaceutical Industry Zongyuan; Ma Shuai; Zhou Weicheng; (7 pag.)CN106928040; (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. 628-21-7, name is 1,4-Diiodobutane, A new synthetic method of this compound is introduced below., category: iodides-buliding-blocks

General procedure: A suspension of alkenyl- or aryl-dithiol(1.0 mmol), triethylamine (2.0 mmol), LR (0.44g, 1.0 mmol) or FcLR (0.56 g, 1.0 mmol) and dihaloalkane(1.0 mmol) in dry THF (60 mL) was stirred under N2 gas atmosphere at ambient temperature for 24 h leadingto a reddish yellow or pale-yellow suspension. Upon filtering to remove insoluble solid the filtrate was driedunder reduced pressure. The residue was dissolved in dichloromethane (ca. 2 mL) and was loaded onto a silicagel column (dichloromethane as eluent) to give the macrocycles. Another unexpected nine-membered ring 4was also obtained in respective 25% and 30% yields in the cases of 5 and 9. Two diastereomers wereseparated completely in the cases of 10 and 12.

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; Hua, Guoxiong; Cordes, David B.; Slawin, Alexandra M. Z.; Woollins, J. Derek; Synlett; vol. 29; 11; (2018); p. 1496 – 1501;,
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. 98-61-3, name is 4-Iodobenzenesulfonyl chloride, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 98-61-3

(R) – [3- [3- (3-fluoro-4-morpholinophenyl) -2-oxo-5-oxazolidinyl] methyl alcohol (3.9 g, 13.16 mmol) ,CH2Cl2, triethylamine (3.67 mL, 26.13 mmol).A solution of p-iodobenzenesulfonyl chloride (15.8 mmol) in CH2Cl2 was added dropwise,Reaction at room temperature for 18 hours.TLC monitoring, the reaction is completed, the reaction solution water washing, saturated NaCl solution washing,Dried over anhydrous Na2SO4, filtered, dried to give the crude product,Recrystallization gave the product (R) -N- [3- (3-fluoro-4-morpholinophenyl) -2-oxo-5-oxazolidinyl] methyl p-iodobenzenesulfonic acidEster 6.1 g,Yield: 82.5%, chemical purity: 98.9%

According to the analysis of related databases, 98-61-3, the application of this compound in the production field has become more and more popular.

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. 755027-18-0, name is 1-Bromo-4-iodo-2-methoxybenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 1-Bromo-4-iodo-2-methoxybenzene

A solution of 1-bromo-4-iodo-2-methoxybenzene (0.63 g, 2.01 mmol) dissolved in toluene (15.7 mL) was treated with 2-methoxy-N-methylethanamine (179 mg, 2.01 mmol), sodium tert-butoxide (232 mg, 2.42 mmol), Xantphos (0.116 g, 0.20 mmol) and tris(dibenzylideneacetaone)dipalladium (0) (46 mg, 0.05 mmol) under a nitrogen atmosphere. The resulting mixture was stirred at 80 C in a sealed tube for 2 hours. The reaction mixture was diluted with water (200 mL), and extracted with EtOAc (200 mL). The organic layerwas dried over MgSO4, filtered and evaporated to afford the crude product. The crudeproduct was purified by flash silica chromatography eluting with 50% Et2O in heptane. Purefractions were evaporated to dryness to afford 4-bromo-3-methoxy-N-(2-methoxyethyl)-Nmethylaniline(231 mg, 42%) as a brown solid.

The synthetic route of 755027-18-0 has been constantly updated, and we look forward to future research findings.

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. 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, A new synthetic method of this compound is introduced below., category: iodides-buliding-blocks

2-methyl-thiophene 3.6g (17.3mmol) at -78C reacted with n-butyl lithium and triethyl borate, 5-methyl-thiophen-2-yl boronic acid to 4.42g (yield: 85%) was formed . 4.42g of 5-methyl-thiophen-2-yl boronic acid react with 5-bromo-2-iodo-benzoic acid methyl ester and 80C by the Suzuki coupling (Suzuki coupling) 7.78g of Intermediate 1 (yield: 80 %) it was synthesized. Intermediate 1 react with CH3MgCl by cyclization (cyclization) with the 3.14g (yield: 40%) intermediate 2 was synthesized . intermediate 2 was reacted with 9-phenyl-anthracene boronic acid and by Suzuki coupling compound 1 (3.3g, yield: 60%) was obtained. Compound 1 was confirmed by 1HNMR and MS.

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

Reference of 98-61-3, 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. 98-61-3, name is 4-Iodobenzenesulfonyl chloride belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

7-PIPSYL-GC (6).; To a suspension of GC (3,99. 8 mg, 0.227 mmol) and 4-iodobenzenesulfonyl chloride (205.7 mg, 0.680 mmol, 3 equiv) in CH2CL2 (2.25 mL) was added pyridine (73 mL, 0.906 mmol, 4 equiv) and the reaction mixture was stirred for 26 h. The solvent was removed under reduced pressure, the residue dissolved in EtOAc and washed with 1M aq. HC1, brine and dried with MGSO4. The crude product was purified by flash column chromatography (gradient 40-99 % EtOAc/hexanes, 1 % AcOH) to obtain 113.8 mg of pure 6 (73% yield) and 24.3 mg of recovered GC (25 %). 1H-NMR (400 MHz, DMSO-d6) 8 8.18-8. 10 (m, 2HA), 7.78-7. 70 (m, 2H), 7.57 (d, J = 5. 5 Hz, 1H, 10- H), 6.52 (s, 1H, 3-OH), 6.13 (s, 1H, 12-H), 5.30 (d, J = 4.2 Hz, 1H, 1-OH), 5.16 (D, J = 4.1 Hz, 1H, 6-H), 5.01 (d, J = 5.5 Hz, 1H, 10-H), 4.85 (dd, J = 12.4, 4.1 Hz, 1H, 7-H), 4. 60 (d, J = 6.5 Hz, 1H, 2-H), 4.09 (dd, J = 6.5, 4.2 Hz, 1H, 1-H), 2.80 (q, J = 7.1 Hz, 1H, 14-H), 1.95 (d, J = 12.4 Hz, 1H, 8- H), 1.10 (d, J = 7.1 Hz, 3H, 16-CH3), 0.98 (s, 9H, tBu) ; 13C- NMR (75 MHz, MEOD) 5 8.16, 29.24, 33.20, 43.17, 50.03, 64.78, 68.71, 70.24, 75.03, 76.67, 81.10, 84.50, 93.47, 100.06, 103.62, 111.14, 130.49, 137.04, 140.39, 171.66, 174.40, 178.05. HRMS (FAB) calcd for C26H28013SI 707.0295, found 707.0265.

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