Month: June 2021

Adding a certain compound to certain chemical reactions, such as: 19821-80-8, name is 1,3-Dibromo-2-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 19821-80-8, category: iodides-buliding-blocks

EXAMPLE 1; Preparation of 5-Bromo-9-isopropylidene-benzonorbornadiene (Compound No. 5.12); a) »-ButvUithium variant, from l,3-dibromo-2-iodo-benzene; To a stirred solution of l,3-dibromo-2-iodo-benzene (5.0Og, 13.8 mmol) and 6,6- dimethylfulvene (7.57g, assay 97%, 69 mmol) in dry toluene (60 ml) under a nitrogen atmosphere 5.5 ml of a 2.5M toluene solution of n-butyllithium (14.5 mmol) were added dropwise at O0C within 10 minutes. After a further 10 minutes at O0C and 1 hour at ambient temperature, the reaction mixture was poured onto a saturated aqueous solution of ammonium chloride, extracted with ethyl acetate, washed with brine and water, dried over sodium sulphate and evaporated. Purification of the crude material on silca gel in hexane afforded 2.55g of the desired product as a yellow oil (assay 99% by g.l.c, 70% yield). Yellow crystals of m.p. 90-910C were obtained from cold hexane.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; SYNGENTA PARTICIPATIONS AG; WO2007/68417; (2007); A2;,
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. 25309-64-2, name is 1-Ethyl-4-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows., Safety of 1-Ethyl-4-iodobenzene

In a 25 mL reaction flask, 3 mL of water, 0.5 mmol of 1-ethyl-4-iodobenzene, 1.0 mmol of DBH, and0.05mmol TBHP, after reacting at 60 C for 4h, add 2.0mmol sodium bicarbonate and 0.5mmol alpha-aminopyridine at 80 CAfter reacting for 2 hours, the reaction mixture was completed, ethyl acetate was added thereto, and brine was added and the organic phase was concentrated.Column chromatography gave 134 mg of a white solid.The yield was 84%.

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 25309-64-2.

Reference:
Patent; Henan Normal University; Zhao Minghao; Ma Chunhua; Zhu Hong; Yang Xiao; Zeng Wenjie; (9 pag.)CN108822106; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 627-31-6, These common heterocyclic compound, 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), 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.

Step-d: 7′-methyl-5′-nitro spirolcyclobutane- 1.3′-indolin1-2′-one: To a stirred solution of 7-methyl-5-nitroindolin-2-one (0.45g, 2.3 mmol) in dry THF was added LiHMDS (7.02 mL, 3 eq) dropwise at 0C and stirred there for 15 min. Subsequently, 1, 3-diiodo propane (1.3 mL, 11.7 mmol) was added and the reaction mixture was stirred at 0C to RT for 2 h. The reaction mixture was quenched with IN HC1. The aqueous layer was extracted with ethyl acetate and washed with water and brine, dried over MgS04 and evaporated. The crude material was purified by column chromatography using 5 % ethyl acetate in hexanes as eluent to afford the title compound as a pale yellow solid (0.060 g, 10%). -NMR (400 MHz, DMSO- d6): 8 10.99 (bs, 1H), 8.29 (d, 8.01 (s, 1H), 2.45-2.41 (m, 4H), 2.28 (s, 3H), 2.25- 2.19 (m, 2H); ES-MS: m z 231.2 (M-H)

Statistics shows that 1,3-Diiodopropane(stabilized with Copper chip) is playing an increasingly important role. we look forward to future research findings about 627-31-6.

Reference:
Patent; ORION CORPORATION; UJJINAMATADA, Ravi Kotrabasaiah; HOSAHALLI, Subramanya; SAMAJDAR, Susanta; ABBINENI, Chandrasekhar; WO2015/92118; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 181765-85-5, 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. 181765-85-5, name is Methyl 4-chloro-2-iodobenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 45Bmethyl 4-chloro-2-(5-(methoxycarbonyl)-2-nitrophenylamino)benzoate 2470 A solution of Example 3 A (5.35 g, 18.04 mmol), methyl 3-amino-4-nitrobenzoate(3.54 g, 18.04 mmol), CsC03 (5.88 g, 18.04 mmol), palladium(II) acetate (0.202 g, 0.902 mmol) and 1 , 1 ‘-bis(diphenylphosphino)ferrocene ( 1.0 g, 1.804 mmol) in toluene was heated at 95C for 16 hours. The reaction mixture was brought to 80C; filtered through a plug of silica gel and washed with ethyl acetate. The solvent was removed and residue 2475 was purified over silica gel. The material was collected and washed with minimumamount of hot ethanol to yield the title compound. MS ESI(+) m/z 365 [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, Methyl 4-chloro-2-iodobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ABBOTT LABORATORIES; ABBOTT LABORATORIES TRADING(SHANGHAI) COMPANY, LTD.; VAN CAMP, Jennifer; PATEL, Jyoti, R.; SWANN, Steven; WO2012/45194; (2012); A1;,
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

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

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 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

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

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