Tag: M.W=200-300

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. 135050-44-1, name is 3-Chloro-4-iodoaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C6H5ClIN

A solution of 3-CHLORO-4-IODO-ANILINE (5. 6G), ISOAMYLNITRITE (8. 8ML) and ETHYLDISULPHIDE (13. 4ML) in acetonitrile (100ml) was heated at 60C for 24h. The solvent was removed under reduced pressure and the residue purified by chromatography on silica eluting with 1% ETHYLACETATE/ISOHEXANE. YIELD 4. 02G ‘H NMR CDC13 : 8 7. 70 (1H, D) ; 7. 36 (1H, d); 6. 87 (1H, dd); 2. 94 (2H, q) ; 1. 32 (3H, t)

The synthetic route of 135050-44-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTRAZENECA AB; WO2004/89885; (2004); A1;,
Iodide – Wikipedia,
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Electric Literature of 83863-33-6, These common heterocyclic compound, 83863-33-6, name is 5-Iodo-2-methylaniline, 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.

9.97 g of N,N-bis(2-chloroethyl)-4-methylbenzenesulfonamide (30.3 mmol) and 5.03 g of potassium iodide (30.3 mmol) in 75 ml. of cyclohexanol were stirred for 1 h at 800C. After addition of 7.7 g of sodium carbonate (72.7 mmol) and 5.65 g of 5-iodo-2-methyl- aniline (24.2 mmol), stirring continued for deltah at 1600C. At room temperature, the mixture was filtered, washed with dichloromethane, and the filtrate evaporated to dryness. The residue was dissolved in dichloromethane, filtered, and the solvent evaporated. The remaining residue was trituated with n-heptane and the crystalline product filtered off, washed several times with n-heptane and dried in vacuo to yield 10.7 g of product

The synthetic route of 83863-33-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ABBOTT GMBH &; CO. KG; ABBOTT LABORATORIES; HAUPT, Andreas; POHLKI, Frauke; DRESCHER, Karla; WICKE, Karsten; UNGER, Liliane; RELO, Ana-Lucia; BESPALOV, Anton; VOGG, Barbara; BACKFISCH, Gisela; DELZER, Juergen; ZHANG, Min; LAO, Yanbin; WO2010/125134; (2010); A1;,
Iodide – Wikipedia,
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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 61272-76-2 as follows. name: 4-Fluoro-2-iodoaniline

General procedure: A 25 mL Wattecs reaction tube was charged with 2-haloaniline 1 (0.6 mmol), potassium O-ethyl dithiocarbonate 2 (1.8 mmol),CuCl (0.06 mmol), and DMF (2 mL). The reaction vessel was flushed with argon three times and sealed. Then the mixture was stirred electromagnetically in an oil bath at 110¡ãC for 6 h.The reaction process was monitored by TLC on silica gel. After the reaction was completed, the reaction mixture was cooled to room temperature, and then HCl (3 mL, 3 mol/L) was added and stirred for another 30 min. The reaction mixture solution was extracted by ethyl acetate (3 ¡Á 20 mL). Subsequently, the combined organic solutions were dried by anhydrous sodium sulfate and the target product was purified by chromatography on a silica gel column (eluent: petroleum ether/ethyl acetate) togive the corresponding pure product 3. Complete characterization characterizationof the products (all known) is found in the Supplemental Materials (Figures S1?S13).

According to the analysis of related databases, 61272-76-2, the application of this compound in the production field has become more and more popular.

Reference:
Article; Liu, Lei; Zhu, Ning; Gao, Min; Zhao, Xiaole; Han, Limin; Hong, Hailong; Phosphorus, Sulfur and Silicon and the Related Elements; vol. 191; 5; (2016); p. 699 – 701;,
Iodide – Wikipedia,
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Application of 77317-55-6, 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. 77317-55-6, name is Methyl 2-amino-5-iodobenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Under an argon atmosphere 200 mg (0.72 mmol) 2-amino-5-iodo-benzoic acid methyl ester is dissolved in 4.0 ml toluene, 156 mg (0.94 mmol) 2-ethoxy-phenylboronic acid, a solution of 475 mg (2.17 mmol) tripotassium phosphate in 0.5 ml water, 53 mg (0.06 mmol) Pd2(dba)3, and 28 mg (0.10 mmol) N-phenyl-2-di-tert.-butylphosphinopyrrole are added. The reaction mixture is heated to 100 C. and stirred over night. After cooling to room temperature the reaction mixture is filterd over celite and the filtrate is evaporated under reduced pressure. The residue is purified by preparative HPLC (eluent A: water+0.13% TFA, eluent B: acetonitrile). The product is dissolved in dichloromethane and extracted with a saturated aqueous solution of Na2CO3. The organic layer is dried and evaporated under reduced pressure. yield: 40 mgRT (Microsorb 1s)=1.72 minESI-MS (M-FH)+=272

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 2-amino-5-iodobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; US2010/249158; (2010); 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. 33348-34-4, name is 4-Amino-3-iodobenzonitrile, A new synthetic method of this compound is introduced below., Product Details of 33348-34-4

To a solution of 4-amino-3-iodobenzonitrile in THF (4 ml.) was added BH3.THF (1 M solution in THF 2.5 ml.) drop-wise. The reaction mixture was refluxed for 3 h and 2 N HCI (1.0 ml.) was added . The resulting mixture was refluxed for an additional 1 h and then concentrated in vacuo in order to afford the crude, which was re-crystallized in MeOH for characterization to give 150 mg (74 %) of yellow powder. 4-amino-3-iodobenzylammonium chloride. ^ NMR (250 MHz, DMF) d 8.90 (s, broad, 3H, +NH3), 7.88 (d, J = 2.0 Hz, 1H, CHar), 7.42 (dd, J = 8.3, 2.1 Hz, 1H, CHar), 6.93 (d, J = 8.3 Hz, 1H, CHar), 5.81 (s, 6H, HCI), 4.06 (q, J = 5.6 Hz, 2H, CH2). (0104) 13C NMR (63 MHz, DMF) d 151.64 (Car-+NH3), 149.11(Car), 140.44 (CHar), 131.17 (CHar), 124.75 (Car), 114.86 (CHar), 82.93(Car-I), 42.30 (CH2).

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; UNIVERSIDAD COMPLUTENSE DE MADRID; FUNDACION PARA LA INVESTIGACION BIOMEDICA DEL HOSPITAL INFANTIL UNIVERSITARIO NINO JESUS; FUNDACION PARA LA INVESTIGACION BIOMEDICA DEL HOSPITAL UNIVERSITARIO LA PRINCESA; VALLET REGI, Maria; BAEZA GARCIA, Alejandro; VILLAVERDE CANTIZANO, Gonzalo; CASTILLO ROMERO, Rafael; RAMIREZ ORELLANA, Manuel; MELEN FRAJLICH, Gustavo; GONZALEZ MURILLO, Africa; ALFRANCA GONZALEZ, Arantzazu; (49 pag.)WO2019/185586; (2019); A1;,
Iodide – Wikipedia,
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Some common heterocyclic compound, 58313-23-8, name is Ethyl-3-iodobenzoate, molecular formula is C9H9IO2, 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 Ethyl-3-iodobenzoate

Ethyl 3-iodobenzoate (0.92 g, 3.34 mmol, 1 eq.), phenylboronic acid (0.87 g, 5.02 mmol, 1.5 eq.), palladium(II)acetate (37 mg, 0.167 mmol, 0.05 eq.) and sodium carbonate (706 mg, 6.66 mmol, 2 eq.) were dissolved in DMF (20 mL) at room temperature under nitrogen. The reaction was then heated at 80 C. for 1.5 hours. Worked up by adding ethyl acetate and rinsing 4 times with water. The organic layer was dried over sodium sulfate and stripped to give a dark oil. Purified over silica gel in 9:1 to 1:1 hexanes/ethyl acetate to obtain 3′-Amino-[1,1′-biphenyl]-3-carboxylic acid, ethyl ester (420 mg) as an oil. Yield=55%. LCMS detects (M+H)+=242.41.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 58313-23-8, its application will become more common.

Reference:
Patent; Carter, Percy H.; Cherney, Robert J.; Batt, Douglas G.; Duncia, John V.; Gardner, Daniel S.; Ko, Soo S.; Srivastava, Anurag S.; Yang, Michael G.; US2005/54627; (2005); A1;,
Iodide – Wikipedia,
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Reference of 33348-34-4, A common heterocyclic compound, 33348-34-4, name is 4-Amino-3-iodobenzonitrile, molecular formula is C7H5IN2, 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.

Description for D20; delta-Cyano-IH-indole^-carboxylic acid (D20); A suspension of 4-amino-3-iodobenzonitrile (2.44 g), 2-oxopropanoic acid (2.64 g), DABCO (3.36 g), and Pd(OAc)2 in DMF (30 ml.) was heated to 105 0C and stirred at that temperature for 1 hour. The solvent was evaporated. EtOAc (200 ml.) was added and the resulting solution was washed with water (100 ml.) and aqueous NaOH solution (20 ml_). The combined aqueous solution was extracted with EtOAc (3 x 150 ml_). The organic fractions were combined. The combined solution was dried over anhydrous magnesium sulfate. The dried solution was concentrated. The residue was triturated to afford 5-cyano-1 /-/-indole-2-carboxylic acid (D20) (1.1 g) as a brown solid.

The synthetic route of 33348-34-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; WO2009/153307; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 1829-28-3, name is Ethyl 2-iodobenzoate, 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 1829-28-3, Product Details of 1829-28-3

To a 2-dram vial with a PTFE-lined cap was charged with acetal 1d (29.4 mg, 0.101 mmol), ethyl 2-iodobenzoate (110 mg, 0.399 mmol), NBE-CO2Me (22.6 mg, 0.149 mmol), Pd(TFA)2 (3.3 mg, 0.00994 mmol), TFA-Gly-OH (3.3 mg, 0.0193 mmol), AgOAc (66.5 mg, 0.398 mmol), and DCE (2.00 mL). The resulting mixture was heated to 100¡ã C. and stirred for 24 h. After cooling to room temperature, ethylenediamine (0.100 mL) was added, and the resulting mixture was stirred at 23¡ã C. for 2 h. The mixture was filtered through a plug of silica gel, eluting with EtOAc (30 mL), and the filtrate was concentrated under reduced pressure. The residue was purified by flash column chromatography (4:1 hexanes/EtOAc eluent) to afford arylation product 3dp (30.8 mg, 69percent yield, Rf=0.33 in 2:1 hexanes/EtOAc) as a light yellow oil. 1H NMR: (400 MHz, CDCl3) delta 8.17 (d, J=8.5 Hz, 1H), 8.04 (s, 1H), 7.83 (d, J=8.1 Hz, 1H), 7.81-7.75 (m, 1H), 7.75-7.68 (m, 1H), 7.60-7.53 (m, 1H), 7.48 (td, J=7.5, 1.3 Hz, 1H), 7.41-7.33 (m, 2H), 7.27 (s, 1H), 7.19 (s, 1H), 7.05 (s, 1H), 6.32 (s, 1H), 5.40 (d, J=13.3 Hz, 1H), 5.23 (d, J=13.3 Hz, 1H), 4.95 (d, J=11.3 Hz, 1H), 4.85 (d, J=11.3 Hz, 1H), 4.05 (q, J=7.1 Hz, 2H), 2.36 (s, 3H), 0.96 (t, J=7.1 Hz, 3H). 13C NMR: (100 MHz, CDCl3) delta 169.2, 159.6, 148.6, 142.4, 141.5, 137.9, 137.5, 131.6, 131.2, 130.80, 130.78, 129.9, 129.7, 129.6, 129.1, 128.8, 128.1, 128.03, 128.01, 127.23, 127.21, 125.7, 103.6, 70.4, 70.1, 61.1, 21.5, 13.9. IR: (film) 1716, 1290, 1248, 1022, 761 cm?1. HRMS: (ESI+) m/z calc’d for (M+H)+ [C28H25NO4+H]+: 440.1856, found 440.1863.

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, Ethyl 2-iodobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; The University of Georgia Research Foundation, Inc; Ferreira, Eric; Li, Qiankun; (47 pag.)US2018/65909; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 696-41-3,Some common heterocyclic compound, 696-41-3, name is 3-Iodobenzaldehyde, molecular formula is C7H5IO, 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: Synthesis of iodo-chrysin derivatives was accomplishedfollowing the general methods shown in Schemes 1 and 2.As outlined in Schemes 1 and 2, under anhydrous andanaerobic conditions, ZnCl2 (0.05 mol) was added to themixture of resorcinol (0.1 mol) and chloroacetonitrile (0.12mol) in diethyl ether (50 mL) cooled to 0C. The mixturewas reacted with anhydrous hydrogen chloride gas for 12hours. Intermediate compound 1, chrysin derivatives 2-5were synthesized according to Scheme 2. The Baker-VenKataraman reaction was employed in the synthesis ofchrysin derivatives [31]. 2, 4-dihydroxybenzoyl chloride (86mmol) was obtained after recrystallization with water. 2-Iodobenzaldehyde, 3-iodobenzaldehyde, 2-fluorine-5-iodobenzaldehyde or 3-iodo-4,5-dimethoxy benzaldehyde(12 mmol) and 10% NaOH (20 mL) were added to a solutionof compound 1 (10 mmol) in alcohol (5 mL). The mixturewas stirred at room temperature for 72 hours. Then the solutionwas acidified with 10% aqueous HCl to pH= 7 andstirred for another 48 hours at room temperature. The crudeproduce was purified by column chromatography (ethylacetate/ petroleum ether = 1:1) to get products, compound2: 7-hydroxy-2-(2-iodophenyl)-4H-chromen-4-one yielded62.7%, compound 3: 7-hydroxy-2-(3-iodophenyl)-4Hchromen-4-one yielded 61.5%, compound 4: 2- (2-fluoro-5-iodo- phenyl)-7-hydroxy-4H-chromen-4-one yielded 60.8%,compound 5:7-hydroxy-2-(3- iodo-4,5-di- methoxyphenyl)-4H-chromen-4-one yielded 62.3%. All compounds were yellowproducts.

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

Reference:
Article; Wei, Yun; Zheng, Qutong; Tang, Guotao; Song, Chen; Wang, Guan; Zhang, Yinxiang; Xiao, Yan; Zeng, Xianliang; Wang, Zongbao; Xiao, Jichang; Zheng, Xing; Medicinal Chemistry; vol. 12; 5; (2016); p. 441 – 447;,
Iodide – Wikipedia,
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These common heterocyclic compound, 5458-84-4, name is 1-Iodo-2-methoxy-4-nitrobenzene, 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. Computed Properties of C7H6INO3

2.00 g (7.17 mmol) of 2-iodo-5-nitroanisole, 2.02 g (14.3 mmol) of (2-fluoropyridin-3-yl)boronic acid (A. Bouillon, J.-C. Lancelot, V. Collot, P. R. Bovy, S. Rault, Tetrahedron 2002, 58, 3323-3328.), 1.81 g (21.5 mmol) of sodium hydrogen carbonate and 117 mg (0.14 mmol) of [1,1′-bis(diphenylphosphino)ferrocene]palladium dichloride are heated to 100 C. in a degassed mixture of 40 ml of dioxane and 10 ml of water for 1 h. After cooling, the mixture is diluted with water and extracted three times with ethyl acetate. The combined organic phases are dried over sodium sulfate, clarified over activated carbon and concentrated. Purification is effected by chromatography on silica gel (eluent: dichloromethane) to obtain 1.55 g (87% of theory) of the desired product. 1H NMR (400 MHz, DMSO-d6, delta/ppm): 3.32 (d, 1H), 8.02 (ddd, 1H), 7.95 (dd, 1H), 7.92 (d, 1H), 7.64 (d, 1H), 7.49 (ddd, 1H), 4.10 (s, 3H). HPLC (Method 6): Rt=3.61 min. MS (ESIpos, m/z): 249 (M+H)+.

The synthetic route of 1-Iodo-2-methoxy-4-nitrobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER SCHERING PHARMA ATIENGESELLSCHAFT; US2010/298293; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com