Tag: M.W=200-300

Synthetic Route of 2142-70-3, 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 2142-70-3 as follows.

A solution of 1-(2-iodophenyl)ethanone (0.86g, 3.49mmol) in THF (l5mL) was treated with trimethylphenylammonium tribromide (1.31g, 3.49mmol) in small portions over 10 minutes at R.T. The resulting yellow suspension was stirred at R.T. for 2 hours. A whiteprecipitate formed and was filtered, washed with diethyl ether and the filtrate was concentrated under reduced pressure to give the crude product. The product was purified by silica column chromatography using Combiflash RF automated purification system (0-100% EtOAc – hexane gradient elution) to give title compound as a yellow oil. The oil was confirmed as desired product by 1H NMR (500MHz ODd3) O 7.97(1 H, d, J=11Hz, ArH), 7.47(2 H, d, J= 8Hz, ArH), 7.18-7.22(1 H, m, J= 4, 12Hz, ArH), 4.47(2 H, 5, CH2Br).

According to the analysis of related databases, 2142-70-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; UNIVERSITY OF DUNDEE; SMITH, Alasdair; HUGGETT, Margaret Jean; SPINKS, Daniel; WOODLAND, Andrew; GILBERT, Ian Hugh; (156 pag.)WO2016/132134; (2016); A1;,
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Application of 52548-14-8, 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. 52548-14-8, name is 2-Iodo-5-methylbenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Step B: Methyl 2-iodo-5-methyl-benzoate The compound of the above Step (6.25 g, 23.9 mmol) is dissolved in anhydrous methanol (100 mL), and then SOCl2 (3.6 mL, 49 mmol) is added dropwise to the well-stirred solution. The solution is refluxed for 18 hours and then evaporated to a volume of 25 mL and then poured into crushed ice (100 g). The resulting mixture is extracted with diethyl ether (2*75 mL). The organic phase is washed with saturated aqueous NaHCO3 solution and then brine, dried over Na2SO4 and evaporated to dryness to yield the title compound.

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

Reference:
Patent; LE TIRAN, Arnaud; LE DIGUARHER, Thierry; STARCK, Jerome-Benoit; HENLIN, Jean-Michel; GUILLOUZIC, Anne-Francoise; DE NANTEUIL, Guillaume; GENESTE, Olivier; FEJES, Imre; TATAI, Janos; NYERGES, Miklos; DAVIDSON, James Edward Paul; MURRAY, James Brooke; CHEN, I-Jen; DURAND, Didier; US2015/31673; (2015); A1;,
Iodide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 116632-39-4, name is 5-Bromo-2-iodotoluene, 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 116632-39-4, Recommanded Product: 116632-39-4

Compound Kl 09 can be synthesized by a person of ordinary skill following Scheme 2 illustrated in FIG. 3. In the first step, compound S2-1 (available for purchase from Acros Organics, CAS No. 86-74-8) is combined with compound S2-2 (available for purchase from Alfa Aesar, CAS No. 116632-39-4), K2C03, and Cul in toluene at 80 C to form compound S2-3, In the second step, compound S2-3 is added to hexanes and cooled to 0 C before dropwise addition of nBuLi, followed by addition of B(OMe)3. The reaction can be allowed to stir before being quenched with aqueous HCl to form compound S2-4. In the third step, compound S2-4 is combined with compound S2-5 (available for purchase from Alfa Aesar, CAS No. 3842-55-5), Pd(OAc)2 and K3P04 in THF at 45 C for 24 hours to form compound Kl 09. It is understood that steps 1 , 2, and 3 can be performed and optimized by a person having ordinary skill in the art without undue experimentation.

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

Reference:
Patent; Harvard College Dean Deng; A ·asipulu-gujike; R ·gemaisi-bomubaleierli; T ·D·xiseer; J ·akuileila-aipalakuilei; R ·P·yadangsi; D ·maikelaolin; D ·K·duweinade; (333 pag.)CN106661001; (2017); A;,
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33348-34-4, name is 4-Amino-3-iodobenzonitrile, 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. name: 4-Amino-3-iodobenzonitrile

Preparation 52; 6-Cyano-2,3,4,9-tetrahydro-lH-carbazol-3-yl)-carbamic acid tert-butyl esterAs described in C Chen et al, J. Org. Chem. (1997) 62, 2676-2677, mix 3- iodo-4-aminobenzonitrile (T. H. Jonckers, et al, J. Med. Chem. 45 (16) 3497-3508 (2002)) (1.3 g, 5.3 mmol) and (4-oxo-cyclohexyl)-carbamic acid tert-butyl ester (3.4 g, 16 mmol) l,4-diazobicyclo[2.2.2]octane (DABCO)(1.8 g, 16 mmol), magnesium sulfate (960 mg, 8 mmol) and DMF (30 mL). Sparge the stirred mixture with nitrogen for 10 min and add palladium(II) acetate (58 mg, 0.26 mmol) and place in a 105 C pre-heated oil bath. After 18 h, cool and dilute with EtOAc. Gravity filter the reaction into a separatory funnel and shake with water/EtOAc. Dry the organic layer (MgSO4) and concentrate to give a dark brown oil. Triturate with hexane (insoluble material is starting ketone). Concentrate the hexane solution and purify by silica gel chromatography (120 g), eluting with methylene chloride (0-40 min), then 10% EtOAc/methylene chloride (40-70 min) to give 550 mg (33%) of an off- white foam. MS (ES): m/z 312 (M+l), 310 (M-I); HPLC: R1 = 2.30 min, (97%).

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

Reference:
Patent; ELI LILLY AND COMPANY; WO2007/2181; (2007); A2;,
Iodide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 612-55-5, name is 2-Iodonaphthalene, 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 612-55-5, Recommanded Product: 612-55-5

General procedure: A 100mL flask was charged with Pd(PPh3)Cl2 (70 mg, 0.1 mmol) and CuI (38 mg, 0.2 mmol). After the flask was evacuated and refilled with argon, NEt3 (20 mL) was added and the suspension was stirred at room temperature. A solution of iodobenzene (10a, 2.04 g, 10 mmol) and propargyl alcohol (616 mg, 11 mmol) in NEt3 (10 mL) was added to the suspension. After the reaction was complete (monitored by TLC), the mixture was filtered through a plug of Celite and washed with EtOAc (20 mL x 3). The combined solution was concentrated and purified by column chromatography on silica gel (Hexane/EtOAc 3:1, v/v) to afford 3-phenylprop-2-yn-1-ol (11a, 1.24 g, 94% yield) as a yellow oil.

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:
Article; Xu, Bin; Gartman, Jackson A.; Tambar, Uttam K.; Tetrahedron; vol. 73; 29; (2017); p. 4150 – 4159;,
Iodide – Wikipedia,
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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. 618-91-7, name is Methyl 3-iodobenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 618-91-7

General procedure: To a solution of 3 (117mg, 1.0mmol), methyl 4-iodobenzoate (288mg, 1.1mmol), Pd(PPh3)2Cl2 (21mg, 0.03mmol), and CuI (5mg, 0.03mmol) in the mixture of THF (20mL) and triethylamine (20mL) was added under a nitrogen atmosphere. After being stirred at 70C for 6h, the solvent was removed under reduced pressure. The residue was purified by silica gel column chromatography with dichloromethane/petroleum ether (1:2, v/v) as the eluent to afford the pure product 5a (221mg, 0.88mmol) as a light brown powder in 88% yield.

The synthetic route of 618-91-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Xu, Zhiqiang; Ge, Haojie; Han, Xie; Liu, Sheng Hua; Meng, Xiang-Gao; Yin, Jun; Tetrahedron; vol. 73; 44; (2017); p. 6386 – 6391;,
Iodide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 19718-49-1, name is Methyl 4-amino-3-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 19718-49-1, HPLC of Formula: C8H8INO2

General procedure: A solution of 2-iodoaniline (333.6 mg, 1.52 mmol, 1.0 equiv) in DCM (5.0 mL) was added with Et3N (0.23 mL, 166.9 mg, 1.65 mmol, 1.1 equiv). The reaction solution was cooled at 0 C and acetyl chloride (0.28 mL, 308 mg, 3.92 mmol, 2.6 equiv) was added into the cooled solution. The resulting mixture was warmed to stir at room temperature overnight. Upon completion, thereaction was added with water and the separated aqueous phase was extracted with EtOAc (3xtimes). The combined organic phases were washed with sat. aq. NaCl, dried over anh. Na2SO4 and concentrated under reduced pressure. The crude material was purified by SiO2 column chromatography eluting with 30% EtOAc-hexane to yield 387.9 mg (98%) of the corresponding N-(2-iodophenyl)acetamide as a white solid.

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:
Article; Chaisan, Nattawadee; Kaewsri, Wilailak; Thongsornkleeb, Charnsak; Tummatorn, Jumreang; Ruchirawat, Somsak; Tetrahedron Letters; (2018); p. 675 – 680;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 340825-13-0, name is 6-Iodo-3,4-dihydronaphthalen-1(2H)-one, 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. Recommanded Product: 340825-13-0

A solution of JR-2-methyl-CBS-oxazaborolidine (MCBSOB, 3.7 mL (3.7 mmoles) 1.0 M in toluene) and borane-diethylaniline complex (BDEA, 7.5 mL, 42 mmoles) in 40 mL toluene was heated to 30. A solution of 6-iodo-3,4-dihydro-2H-naphthalen-l-one (10 grams,36.8 mmoles) in 40 mL toluene was added dropwise over 2.5 hours. The reaction mixture was stirred for an additional 0.5 hour at 30. To the solution (at room temperature) was added 20 mL methanol. After 0.25 hour, 50 mL IN hydrochloric acid was added slowly. The mixture was stirred for 20 minutes then it was extracted with 200 mL ethyl ether. The organic phase was washed with IN hydrochloric acid, water, and saturated sodium chloride . The organic phase was dried (magnesium sulfate) and concentrated under reduced pressure. To the oily residue was added 100 mL hot hexane. When crystallization was complete, the white solid was collection and dried to give S-6- iodo-l,2,3,4-tetrahydro-naphthalen-l-ol, 9.62 grams (95%). m.p. 102-103, M+’ = 274, [alpha]D = +12.2 (c = 1, chloroform).

The synthetic route of 6-Iodo-3,4-dihydronaphthalen-1(2H)-one has been constantly updated, and we look forward to future research findings.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; WO2006/66790; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 104539-21-1, 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. 104539-21-1 name is 1-Iodo-2-(2-methoxyethoxy)ethane, 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: Individual solutions of N-(trimethylsilyl)methyl-N-benzylamine (15.5 mmol) in MeCN (100 mL) containing K2CO3 (31 mmol) and alkyl halide (30 mmol of 1-hexyl bromide, 2-(2-methoxyethoxy)ethyl iodide, ethyl 2-bromopropionate) were stirred for 12 h at room temperature and concentrated in vacuo to give residues that were triturated with CH2Cl2. The triturates were dried and concentrated in vacuo to afford residues, which were subjected to column chromatography (EtOAc: Hex=1: 8) to yield 19 (81 %), 22 (90 %) and 23 (44 %).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Iodo-2-(2-methoxyethoxy)ethane, and friends who are interested can also refer to it.

Reference:
Article; Lim, Suk Hyun; Cho, Dae Won; Mariano, Patrick S.; Tetrahedron; vol. 74; 3; (2018); p. 383 – 391;,
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. 5876-51-7, name is 5-Iodobenzo[d][1,3]dioxole belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 5-Iodobenzo[d][1,3]dioxole

General procedure: CuI (10mol%) and EDA (10mol%) were added to a mixtureof O-alkyl carbamate (1mmol), NaOtBu (1.5mmol) and aryl halide (1mmol) in 2mL toluene and the mixture wasstirred for the appropriate time, which was determined byTLC monitoring, at 100C. After completion of the reaction,the catalyst was removed by filtration and 20mL H2Owas added to the filtrate. The resultant mixture was extractedwith CHCl3.Then the organic phase was washed with water(2 × 10mL) and dried over anhydrous Na2SO4.After evaporationof CHCl3under reduced pressure, the correspondingcrude product was purified by flash chromatography to givethe desired pure cross-coupling product in good to excellentyield. In the case of using arylboronic acids as couplingpartners, Cu(OAc)2 was employed instead of CuI.

The synthetic route of 5876-51-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Sardarian, Ali Reza; DindarlooInaloo, Iman; Zangiabadi, Milad; Catalysis Letters; vol. 148; 2; (2018); p. 642 – 652;,
Iodide – Wikipedia,
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