Author: Jessica.F

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. 16355-92-3, name is 1,10-Diiododecane, A new synthetic method of this compound is introduced below., Safety of 1,10-Diiododecane

EXAMPLE 22 N, N’-Decane-1, 10-diyl-bis-nicotinium Diiodide (bNDI).; S- (-)-Nicotine (30.8 mmol) was dissolved in glacial acetic acid (35 mL) and the solution was stirred at ambient temperature for 5 minutes. 1, 10-Diiododecane (15.4 mmol) was added to the solution and the mixture stirred and refluxed for 3 days. The mixture was then evaporated under reduced pressure to remove the solvent and the resulting oil was treated with an aqueous mixture of sodium bicarbonate. The aqueous mixture was extracted with ethyl ether (3 x 50 mL) and chloroform (3 x 50 mL) and the aqueous layer collected and was evaporated to dryness on a rotary evaporator, and the resulting solid was treated with chloroform and filtered. The filtrate was collected and evaporated to dryness. The resulting yellow oil was isolated in a 27% yield. ‘H NMR (300 MHz, CDC13) 8 9.55 (1H, s, C2-H), 9.44 (1H, d, C6-H), 8.53 (1H, d, C4-H), 8.09 (1H, m. C3-H), 4.98 (2H, t, C”1-CH2), 3.74 (1H, t, pyrolidine CH2), 3.30 (1H, t, pyrrolidine CH2,2. 50 (2H, m, C”2-CH2), 2.29 (3H, s, pyrrolidine N-CH3), 1.65-2. 20 (SH, m, pyrrolidine CH2CH2), 1.30-1. 57 (6H, m, C”3-5-CH2); 13C NMR (75 MHz, CDC13) 8 146.6, 143.9 x 2, 143.4, 128.4, 66.9, 61.9, 57.0, 40.8, 36.1, 32.1, 28.5, 28.2, 25.8, 23.5.

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; UNIVERSITY OF KENTUCKY RESEARCH FOUNDATION; WO2005/66129; (2005); A2;,
Iodide – Wikipedia,
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Related Products of 19094-56-5, 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. 19094-56-5, name is 2-Chloro-5-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

2-Chloro-5-iodobenzoic acid (10.0 g, 35.3 mmol) And suspended in methylene chloride (200 mL). N, N-Dimethylformamide (0.05 mL) was added to the resulting mixture, followed by the dropwise addition of oxalyl chloride (11.3 g, 89.0 mmol) at 0 C. After completion of the dropwise addition, the resulting mixture was allowed to warm to room temperature and stirred for 4 hours. The resulting clear solution was evaporated by rotary evaporation to remove the solvent and yielded 10.7 g of product in 100% yield, which was used directly in the next reaction without purification.

The synthetic route of 2-Chloro-5-iodobenzoic acid has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SENJU Pharma Corporation Limited; Woo, Frank; (28 pag.)KR2015/81220; (2015); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 58313-23-8, The chemical industry reduces the impact on the environment during synthesis 58313-23-8, name is Ethyl-3-iodobenzoate, I believe this compound will play a more active role in future production and life.

General procedure: To a dried sealed vessel was added 1,2,3,4-tetrahydroisoquinoline (5 mL, 40 mmol), anhydrous K2CO3 (8.34 g,60 mmol), CuI (0.8 g, 4 mmol), L-Proline (0.92 g, 8 mmol), ethyl 6-bromopicolinate (4.32 g, 20 mmol), and DMSO (25 mL). Then themixture was stirred at 80 C for 16 h under N2 environment. Aftercooling to room temperature, water (100 mL) was added andextracted with EtOAc. Then, the combined organic layer was driedover MgSO4, filtered, and concentrated. The residue was purified bysilica gel flash chromatography (hexane/EtOAc = 5/1) to providecompound 14 as a white oil (3.94 g, 70%).

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-3-iodobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Fang, Yuying; Zhou, Huihao; Gu, Qiong; Xu, Jun; European Journal of Medicinal Chemistry; vol. 167; (2019); p. 133 – 145;,
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. 167479-01-8, name is tert-Butyl (3-iodopropyl)carbamate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 167479-01-8

Part C A solution of 4-amino-2-ethoxymethyl-1-isopropylamino-1H-imidazo[4,5-c]quinolin-7-ol (0.11 g, 0.35 mmol) in 10 ML of N,N-dimethylformamide was placed under an atmosphere of nitrogen and was treated with cesium carbonate (0.23 g, 0.70 mmol).After 5 min of stirring the mixture was treated with tert-butyl 3-iodopropylcarbamate (0.12 g, 0.35 mmol) and heated to 65 C. After 60 h, the reaction mixture was cooled to ambient temperature and then poured into 100 ML of ice water which resulted in a cloudy suspension.The mixture was extracted with CHCl3 (5*25 ML).The combined organic extracts were then washed with brine (50 ML), dried over Na2SO4, filtered and concentrated under reduced pressure to yield a tan oil.Chromatography (95:5 CHCl3:(80:18:2 CHCl3:MeOH:NH4OH) gradient to 1:1 gave 0.040 g of [3-(4-amino-2-ethoxymethyl-1-isopropylamino-1H-imidazo[4,5-c]quinolin-7-yloxy)propyl] tert-butyl carbamate as a light tan solid. LC/MS (APCI) m/z 473 (M+H)+.

The synthetic route of 167479-01-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; 3M Innovative Properties Company; US2004/176367; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 40400-15-5,Some common heterocyclic compound, 40400-15-5, name is 2-(2-Iodophenyl)acetonitrile, molecular formula is C8H6IN, 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: A flask was equipped with a magnetic stir bar and charged with 1Hpyrrole-2-carbaldehyde (2a; 19.0 mg, 0.2 mmol, 1.0 equiv), 2-bromophenylacetonitrile(1a; 39.2 mg, 0.2 mmol, 1.0 equiv), and K3PO4(63.6 mg, 0.3 mmol, 1.5 equiv). The flask was evacuated and filledwith N2, and then anhydrous DMSO (2.0 mL) was introduced via a syringe.The flask was heated in a 130 C oil bath for 24 h, at which timeTLC analysis [petroleum ether (bp 60-90 C)-EtOAc, 10:1] indicatedcomplete consumption of 2a and 1a. The reaction mixture was cooledto r.t. and added to a sat. solution of NaCl (20 mL) and extracted withEtOAc (3 × 10 mL). The combined organic layers were dried (Na2SO4)and filtered. The filtrate was concentrated, and the residue was purified by column chromatography on SiO2 [petroleum ether (bp 60-90C)-EtOAc, 10:1 to 30:1] to give 3am; Yield: 27.9 mg (67%); tan solid; mp 191.3-192.0 C.

The synthetic route of 40400-15-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Jiang, Zeng-Qiang; Miao, Da-Zhuang; Tong, Yao; Pan, Qiang; Li, Xiao-Tong; Hu, Ren-He; Han, Shi-Qing; Synthesis; vol. 47; 13; (2015); p. 1913 – 1921;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

82998-57-0, name is 3-Iodo-4-methylbenzoic acid, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Recommanded Product: 82998-57-0

Oxalyl chloride (1.739 g, 1.20 ml, 13.7 mmol) was added dropwise to a solution of 3-iodo-4-methyl benzoic acid (0.717 mg, 2.74 mmol) and dichloromethane (9 ml). N,N-dimethylformamide (1 drop) was added and the colorless solution stirred at room temperature for 1 h. The solution was concentrated to afford 3-iodo-4-methyl benzoyl chloride as a light yellow solid which was used without purification. 2-(4-amino-2-(trifluoromethyl)benzyl)isoindoline-1,3-dione (Ic) (0.922 g, 2.88 mmol) was added to a solution of 3-iodo-4-methyl benzoyl chloride (0.767 g, 2.74 mmol) in dichloromethane (5 ml) and the mixture stirred at room temperature for 30 min. Triethylamine (0.360 g, 0.50 ml, 3.56 mmol) was added and the solution stirred at room temperature for 1 h. The reaction mixture was partitioned between dichloromethane and saturated aqueous sodium bicarbonate solution. The aqueous phase was separated and extracted with dichloromethane. The combined organic phases were washed with water, brine, dried over anhydrous sodium sulfate, filtered and concentrated to afford a solid (N-(4-((1,3-dioxoisoindolin-2-yl)methyl)-3-(trifluoromethyl)phenyl)-3-iodo-4-methylbenzamide (Id)).

The synthetic route of 82998-57-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Apicore, LLC; Kovi, Ravishanker; Kannapan, Jayaraman; Thakor, Sanjay F.; Patel, Rajesh A; US2014/343282; (2014); A1;,
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 13421-13-1 as follows. Formula: C7H4ClIO2

3.35 g (153.18 mmol) of methyl 4,5-dimethyl-1H-pyrrole-3-carboxylate prepared in accordance with the literature (Synthetic uses of tosylmethyl isocyanide (TosMIC) Organic Reactions (Hoboken, N.J., United States) (2001), 57, No 418) and 4.63 g (16.4 mmol) of 4-chloro-2-iodo-benzoic acid are dissolved in 50 mL of acetonitrile. There are added thereto copper powder (45 (280 mg, 4.37 mmol) as well as caesium carbonate (14.25 g, 43.74 mmol). The reaction mixture is heated at reflux for 12 hours. The progress of the reaction is monitored by liquid chromatography (LC). The suspension is allowed to return to ambient temperature and is then filtered, washed with acetonitrile and evaporated to dryness. The residue is taken up in ethyl acetate. The solution is then washed with 1M hydrochloric acid and then with a saturated sodium chloride solution, it is dried over maganesium sulphate, filtered and then evaporated to dryness. The compound so obtained is purified over a silica gel column using dichloromethane and ethanol as solvents. (0126) Mass spectroscopy (ESI+): (0127) Empirical formula: C15H14ClNO2 (0128) monoisotopic mass=307.07 Da (0129) [M+H]+, measured: 308.12 (0130) (isotope ratios consistent with one chlorine atom)

According to the analysis of related databases, 13421-13-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Les Laboratoires Servier; Vernails (R&D) Limited; CASARA, Patrick; LE DIGUARHER, Thierry; HENLIN, Jean-Michel; STARCK, Jeroeme-Benoit; LE TIRAN, Arnaud; DE NANTEUIL, Guillaume; GENESTE, Olivier; DAVIDSON, James Edward Paul; MURRAY, James Brooke; CHEN, I-Jen; WALMSLEY, Claire; GRAHAM, Christopher John; RAY, Stuart; MADDOX, Daniel; BEDFORD, Simon; (72 pag.)US2016/152599; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 6940-76-7, 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 6940-76-7 as follows.

Anhydrous potassium carbonate (10.6 g, 6 eq) was added to a solution of 4-chloro-7-hydroxy-6-methoxyquinoline-3-carbonitrile (3 g,12.7 mmol) in DMF (30 mL)After stirring for half an hour,1-Chloro-3-iodopropane (13 g, 63.9 mmol) was added to the suspension and stirred at room temperature overnight.The reaction solution was diluted with water (500 mL)Dichloromethane extraction (250 mL X2),The organic phases were combined,Respectively, with water,Washed with a saturated saline solution,Dried over anhydrous sodium sulfate,filter,Concentrated under reduced pressure,Silica gel column chromatography gave 4-chloro-7- (3-chloro-propoxy) -6-methoxy-quinoline-3-carbonitrile (yellow solid, 3.1 g)Yield 77%.

According to the analysis of related databases, 6940-76-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Shanghai Pharmaceuticals Holding Co., Ltd.; Wan, huixin; Shen, JingKang; Li, ChunLi; Han, yanan; Liu, Haiyan; Zhou, ZhaoLi; Li, Ping; Li, Yufeng; Chen, gang; Xu, Jia; (54 pag.)CN103848785; (2016); B;,
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. 153898-63-6, name is 2-Iodo-5-methoxyaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C7H8INO

General procedure: Bis(triphenylphosphine)palladium(ll) dichloride (32.1 mg, 45.8 muiotatauiotaomicronIota), copper(l) iodide (17.8 mg, 91 .5 muiotatauiotaomicronIota), 2-iodo-5-methoxyaniline (1 .2 g, 4.6 mmol), phenylacetylene (572.5 ml, 5.5 mmol), and diethylamine (10 ml) are refluxed until consumption of the starting materials monitored by TLC. The residue is chromatographed on silica gel (heptane/EE, 10/1 ) to afford 5- Methoxy-2-(phenylethynyl)aniline (818 mg, 3.7 mmol, 80 % of theory).1 H NMR (500 MHz, Chloroform-d) delta 7.54 (d, J = 6.7 Hz, 2H), 7.36 (q, J = 8.9 Hz, 7.7 Hz, 2H), 7.32 (q, J = 8.9 Hz, 8.5 Hz, 2H), 6.34 (dd, J = 8.5 Hz, 2.4 Hz, 1 H), 6.30 (d, J = 2.3 Hz, 1 H), 3.82 (s, 3H).

The synthetic route of 153898-63-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK PATENT GMBH; SCHRAUB, Martin; DOBELMANN-MARA, Lars; RIEDMUELLER, Stefan; (326 pag.)WO2018/149852; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 619-58-9, 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. 619-58-9, name is 4-Iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a test tube containing a magnetic bar was added aryl halide (1.0 mmol), CuCl2 (13.4 mg, 0.1 mmol), KOH (336 mg, 6.0 mmol), ethylene glycol(12 muL, 0.2 mmol), and DMSO/H2O (1.0 mL/0.5 mL). After flushing with argon, the mixture was stirred in a preheated oil bath at 120 C for 24 h. After cooled to ambient temperature, the reaction mixture was distributed in aqueous HCl (5 %) and ethyl acetate. The organic layer was washed with water and brine, dried over anhydrous MgSO4, and concentrated under vacuum. The crude product was further purified by column chromatography (EtOAc/n-Hexane) to provide the phenols.

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, 4-Iodobenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Kim, Jihye; Battsengel, Oyunsaikhan; Liu, Yajun; Chae, Junghyun; Bulletin of the Korean Chemical Society; vol. 36; 12; (2015); p. 2833 – 2840;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com