Tag: M.W=200-300

Adding a certain compound to certain chemical reactions, such as: 620-05-3, name is (Iodomethyl)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 620-05-3, COA of Formula: C7H7I

General procedure: A mixture of 4-oxo-1,4-dihydroquinoline-2-carboxylic acid alkylester (1, 1 mmol), base (1.3 mmol), the corresponding alkylatingagent (alkyl iodide, 1.5 mmol; others, 1.2 mmol) and anhydrousDMF (5 mL) was stirred at the appropriate temperature andmonitored by TLC (DCM:MeOH 4.7:0.3). After a specified time(Table 2), the mixture was carefully poured into ice-water. Thecompounds obtained were isolated and purified as was indicatedabove. Alkylating agents, bases and solvents are presented inTable 2.

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, (Iodomethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Shmidt, Maria S.; Arroyo Manez, Pau; Stortz, Carlos A.; Perillo, Isabel A.; Vega, Daniel; Blanco, Maria M.; Journal of Molecular Structure; vol. 1128; (2017); p. 142 – 150;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 19099-54-8, A common heterocyclic compound, 19099-54-8, name is 1-Iodo-2-isopropylbenzene, molecular formula is C9H11I, 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.

0.3 mmol of sodium carbonate, N-(3-(4-methoxyphenyl)prop-2-yn-1-yl)-4-methylbenzenesulfonamide0.1mmol,Tetrakis(triphenylphosphine palladium) 0.005 mmol, bis(2-diphenylphosphinophenyl)ether 0.005 mmol,0.2 mmol of 4-methylbenzeneboronic acid, 0.3 mmol of 2-isopropyliodobenzene, and 1 mL of N,N-dimethylformamide were added to a 15 mL reaction tube.Nitrogen was repeatedly filled 10 times, placed in an oil bath at 120 C, and reacted for 24 hours;Cooled to room temperature, the reaction was diluted with ethyl acetate, washed with water three times, the organic phase dried over anhydrous Na2SO4, filtered, and concentratedPurification by thin layer chromatography to give 21.5mg of the desired product, yield 41%.

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; Huaqiao University; Cheng Guolin; Lv Weiwei; (20 pag.)CN109879713; (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. 10297-05-9, name is 1-Chloro-4-iodobutane, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C4H8ClI

(Step 2) [1-(2-Hydroxyethyl)imidazolidin-2-ylidene] malononitrile (2.00 g, 11.2 mmol) obtained in the Step 1 was dissolved in DMF (20 mL) and the solution was sequentially added with potassium carbonate (3.10 g, 22.4 mmol) and 1-chloro-4-iodobutane (2.75 mL, 22.4 mmol). After stirring the mixture at room temperature for 71 hours, potassium carbonate (3.10 g, 22.4 mmol) and 1-chloro-4-iodobutane (2.75 mL, 22.4 mmol) were added, followed by stirring at 35°C for 6 hours and at a room temperature for 14 hours. The mixture was added with water and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and the solvent was evaporated under reduced pressure. The residue was washed with diisopropylether to obtain [1-(4-chlorobutyl)-3-(2-hydroxyethyl)imidazolidin-2-ylidene]malononitrile (2.55 g, 84.6percent) as a white solid. 1H NMR (CDCl3, deltappm): 1.87-1.99 (m, 2H), 2.12-2.24 (m, 2H), 3.61-3.76 (m, 12H).

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 10297-05-9.

Reference:
Patent; KYOWA HAKKO KOGYO CO., LTD.; EP1847530; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 216393-67-8, 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 216393-67-8 as follows.

4~Chloro-2-fluoro-6-iodoaniline (Intermediate 30, 1.35 g, 5 mmol), pyruvic acid (1.32 g,15 mmol) and DABCO (1.68 g,15 mmol) were dissolved in DMF(15 mL). The solution was degassed and palladium acetate (56 mg) was added. The mixture was then heated to 1000C for 3h., cooled to ambient and filtered. The filtrate was diluted with EtOAc (100 mL), washed with 2M HCl (2 x 2OmL), water (20 mL) and brine (20 mL), dried (MgSO4) and evaporated to leave the title compound as a dark solid (0.9g, 85% ). 1H NMR (400 MHz, DMSO-de) delta 7.16 (IH, t), 7.21 – 7.24 (IH, m), 7.59 (IH, d), 12.52 (IH, s), 13.27 (IH, s); MS m/z 212 (M-H)”

According to the analysis of related databases, 216393-67-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2006/82400; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 3210-08-0,Some common heterocyclic compound, 3210-08-0, name is 4-Iodobutan-1-ol, molecular formula is C4H9IO, 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.

Method A: A solution of [PP(I)P] (215 mg, 0.292 mmol) in THF(10 mL) was added to a stirring suspension of CuI (55.6 mg,0.292 mmol) in THF (5 mL). The cloudy orange reaction mixturewas allowed to stir overnight at 50 C and then filtered throughCelite to obtain an orange filtrate. Removal of the volatiles fromthe filtrate in vacuo afforded analytically pure product as a paleorange solid (88.7 mg, 30% yield).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-Iodobutan-1-ol, its application will become more common.

Reference:
Article; Knight, Sadie E.; Bezpalko, Mark W.; Foxman, Bruce M.; Thomas, Christine M.; Inorganica Chimica Acta; vol. 422; (2014); p. 181 – 187;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 618-91-7, 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. 618-91-7, name is Methyl 3-iodobenzoate, This compound has unique chemical properties. The synthetic route is as follows.

3(ii) 3-Trimethylstannyl-benzoic acid methyl ester (3)Microwave 2 3To a mixture of methyl 3-iodobenzoate 200 mg, 0.76 mmol), and hexamethylditin (643 mul, 3.1 mmol) in toluene (8 ml) was added tetrakis (triphenylphosphine) palladium (0) (180 mg, 0.155 mmol (10 mol %). The reaction tube was flushed with argon, capped and heated in a microwave at 120C for 15 minutes. After cooling, TLC (ethyl acetate/hexane, 1 :1 ) showed complete conversion to product. Then the black suspension was filtered (filter paper) and the resulting dark coloured solution was evaporated to dryness. The residue was dissolved in ethyl acetate (15 ml) and extracted with water (6×10 ml).Then the organic phase was dried (MgSO4) filtered and evaporated under reduced pressure to afford the crude product as a dark oil (463 mg) which was purified by flash chromatography (Ethyl acetate: hexane, 1 :1 ) to afford a slightly yellow oil. Yield: 344 mg (74%).NB: Microwave irradiation was carried out in a Personal Chemistry Emrys synthesizer.1H NMR (500 MHz, CDCI3, £0.32 (s, 9H, Sn(CH3)3, 3.95(s, 3H, CH3), 7.40 (t, 1 H), 7.69 (d, 1 H), 8.0 (d 1 H), 8.20 (s, 1 H)

The chemical industry reduces the impact on the environment during synthesis Methyl 3-iodobenzoate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; GE HEALTHCARE LIMITED; AVORY, Michelle; BROWN, Jane; IVESON, Peter Brian; WO2010/86398; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 117832-17-4, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 117832-17-4 name is 2-Iodo-4,5-dimethylaniline, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

General procedure: 2-iodoaniline (54.8 mg, 0.25 mmol) 1a, sodium azide (19.5 mg, 0.3mmol) 3, CuI (4.8 mg, 0.025 mmol), K2CO3 (34.5 mg, 0.25 mmol),phenylacetaldehyde (58 muL, 0.5 mmol) 2a, (DMEDA) (3 muL, 0.025mmol) were taken in a round bottom flask equipped with stirrer in 1.0mL of DMSO. The reaction mixture was heated to 80 C for 20 h.After cooling the room temperature, to the reaction mixture wasadded water (2 mL), and extracted with EtOAc (310 mL). Thecombined organic phases were washed with brine (25 mL), driedover anhydrous MgSO4 and concentrated in vacuo. The residue wassubjected to flash column chromatography with petroleum/ethylacetate (20/1) to afford the final product 4aa as light yellow solid

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Iodo-4,5-dimethylaniline, and friends who are interested can also refer to it.

Reference:
Article; Yuan, Hua; Li, Kangning; Chen, Yongxin; Wang, Yu; Cui, Jiaojiao; Chen, Baohua; Synlett; vol. 24; 17; (2013); p. 2315 – 2319;,
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 31599-61-8 as follows. SDS of cas: 31599-61-8

General procedure: To the catalyst (1.0mol%) dissolved in 10ml THF in a 25ml round-bottom flask, aryl halide (1.0mmol), phenyl boronic acid (1.2mmol) and K2CO3 (2.0mmol) were all added. The mixture was stirred at refluxing temperature for 4h. After completion of the reaction, the mixture was evaporated to dryness, water was added and the product was extracted with dichloromethane. The organic layer was washed with brine, dried over Na2SO4, filtered, passed through a silica column (60-120 mesh), where the complex remained trapped. Upon removal of the solvent, pure solid products were obtained. The yields of the products obtained (based on the aryl halides) from all the reactions were determined after isolation, and the products were characterized by 1H NMR spectra and melting points by a comparison with the literature data.

According to the analysis of related databases, 31599-61-8, the application of this compound in the production field has become more and more popular.

Reference:
Article; Pratihar, Jahar Lal; Mandal, Paritosh; Lin, Chia-Her; Lai; Mal, Dasarath; Polyhedron; vol. 135; (2017); p. 224 – 230;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 58755-70-7, A common heterocyclic compound, 58755-70-7, name is 1-Iodo-4-methoxy-2-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.

General procedure: To a degassed solution of 2-(6-trimethylsilyl-3(Z)-hexen-1,5-diynyl)-1,2,3-trimethoxybenzene (15) (12 mmol) containing CuI (3.2 mmol) and K2CO3 (30 mmol) in MeOH (15 ml) was added a degassed solution of aryl iodides (16a-i) (12 mmol) containing Pd(PPh3)4 (0.8 mmol) in MeOH (20 ml). The resulting reaction mixture was stirred at room temperature for 4 h. The solvent was then removed in vacuo. The residue was quenched with saturated aqueous NH4Cl and extracted with EtOAc (20 × 3 ml). The combined organic extracts were washed with saturated aqueous Na2CO3 (40 ml) and dried over anhydrous MgSO4. After filtration and removal of the solvent in vacuo, the residue was purified by column chromatography on a silica gel to produce the desired products

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; Lo, Yu-Hsiang; Lin, Ying-Ting; Liu, Yu-Peng; Duh, Tsai-Hui; Lu, Pei-Jung; Wu, Ming-Jung; European Journal of Medicinal Chemistry; vol. 62; (2013); p. 526 – 533;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 2401-21-0, name is 1,2-Dichloro-3-iodobenzene, 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 2401-21-0, Application In Synthesis of 1,2-Dichloro-3-iodobenzene

1.68 g of 17-(m-iodobenzoyloxy)-3-oxo-androst-4-ene-17beta-carboxylic acid and 825 mg of iodobenzene dichloride were gasified with argon in 340 ml of chloroform and exposed for 20 minutes with a mercury high-pressure lamp. The solution was washed with dilute sodium bisulphite solution and water, dried and evaporated in vacuo. Chromatography on silica gel gave 9alpha-chloro-17-(m-iodobenzoyloxy)-3-oxo-androst-4-ene-17beta-carboxylic acid of melting point 236°-237° C.; [alpha]D =-40° (dioxan, c=0.1percent); epsilon220 =34,900.

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, 1,2-Dichloro-3-iodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Hoffmann-La Roche Inc.; US4252729; (1981); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com