Month: July 2021

Application of 624-75-9, 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 624-75-9 as follows.

EXAMPLE 163 4-Chloro-N-[(3RS,4SR)-4-(4-chloro-phenyl)-1-(1-cyanomethyl-piperidine-4-carbonyl)-pyrrolidin-3-yl]-N-methyl-3-trifluoromethyl-benzamide To a solution of 4-chloro-N-[(3RS,4SR)-4-(4-chloro-phenyl)-1-(piperidine-4-carbonyl)-pyrrolidin-3-yl]-N-methyl-3-trifluoromethyl-benzamide (216 mg, 0.382 mmol) in DMF (1 mL) was added sodium hydride (55% dispersion in mineral oil, 6 mg, 0.14 mmol). After stirring for 30 min at ambient temperature iodoacetonitrile (9 mul, 0.12 mmol) was added And the suspension was stirred for 18 h at this temperature. After the addition of further iodoacetonitrile (9 mul, 0.12 mmol) the resulting dark brown solution was stirred for further 5 h at ambient temperature. It was diluted with ethyl acetate (10 mL) and was washed with aqueous sodium carbonate (1 M, 10 mL) and brine (10 mL). The aqueous layers were extracted with ethyl acetate (10 mL) and the combined organic phases were dried over sodium sulfate. Purification by chromatography (SiO₂, (ethyl acetate_triethylamine=95:5):methanol=100:0 to 70:30) afforded the title compound (45 mg, 88%) as a white foam. MS m/e: 567.1 [M]⁺.

According to the analysis of related databases, 624-75-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Bissantz, Caterina; Jablonski, Philippe; Knust, Henner; Koblet, Andreas; Limberg, Anja; Nettekoven, Matthias; Ratni, Hasane; Riemer, Claus; US2009/312327; (2009); A1;,
Iodide – Wikipedia,
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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. 14452-30-3, name is 1-(3-Iodophenyl)ethanone, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 14452-30-3

General procedure: All the chemicals and solvents were purchased from Sigma Aldrich. The progress of all reactions was monitored on Merck KGaA precoated silica gel plates 0.25 mm (with fluorescence indicator UV254) using ethyl acetate/n-hexane as solvent system. Spots were visualized by irradiation with ultraviolet light (254 nm). Melting points (mp) were determined using open capillary method on Melting Point III Marte apparatus. Proton (1H) and (13C) NMR spectra were recorded on Bruker Avance 400 spectrometer at 400 MHz for 1H and 100 MHz for 13C using DMSO-d6 and CDCl3 as solvents referenced. Chemical shifts are given in parts per million (ppm) (delta relative to residual solvent peak for 1H and 13C). Spectra Mass was performed on a LCMS-2020 Liquid Chromatograph Mass Spectrometer Shimadzu, the column was Agilent XDB-C18, 35 muM, 21×20 nm. IR spectra were recorded on a PerkinElmer model Spectrum 400 (medium, sweep of 4000 to 400 cm-1). Synthesized compounds were ?96% pure as determined by high performance liquid chromatography (HPLC) Shimadzu with PDA detector, Nucleodur 100-5 CN-RP column 205×4.6mm, mobile phase water/0.1% TFA and acetonitrile with flow of 1mL/min. For the synthesis of 3-25, substituted acetophenones (0.5 equiv, 0.5 mmol) and nitroaromatics (0.5 equiv. 0.5 mmol) were dissolved in acetic acid (1mL) and concentrated sulfuric acid (0.05 mL) and were stirred at 100C until completion of the reaction (4-24h). The cooled mixture and the solid was washed with iced methanol (200 mL) for purification. For the synthesis of 26-35, 0.4 mL of aqueous NaOH (20% w/v) was added to the solution of the acetophenones substituted in 4? position (1 mmol) in EtOH. The resulting mixture was stirred at the room temperature for 10 h. The formed precipitate was filtered and washed with cold water. If no precipitation occurred, the resulting mixture was neutralized with 5% HCl filtered and dried. The crude was then subjected to chromatography column with EtOAc/Hexane (7:3, v/v) as eluent.

According to the analysis of related databases, 14452-30-3, the application of this compound in the production field has become more and more popular.

Reference:
Article; Gomes, Marcelo N.; Braga, Rodolpho C.; Grzelak, Edyta M.; Neves, Bruno J.; Muratov, Eugene; Ma, Rui; Klein, Larry L.; Cho, Sanghyun; Oliveira, Guilherme R.; Franzblau, Scott G.; Andrade, Carolina Horta; European Journal of Medicinal Chemistry; vol. 137; (2017); p. 126 – 138;,
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. 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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Application of 144-48-9, 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. 144-48-9, name is 2-Iodoacetamide belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

1) To a solution (10 mL) of 5- { [ (tert- butoxycarbonyl) amino] methyl}-6-isobutyl-2-methyl-4- (4- methylphenyl) nicotinic acid (500 mg, 1.22 mmol) in N, N- dimethylformamide were added 2-iodoacetamide (673 mg, 3.64 mmol) and potassium carbonate (337 mg, 2.44 mmol) and the mixture was stirred at room temperature for 30 min. The reaction mixture was diluted with ethyl acetate (100 mL) and washed with saturated brine. The organic layer was dried over anhydrous magnesium sulfate and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to give 2-amino-2-oxoethyl 5- { [ (tert-butoxycarbonyl) amino] methyl}-6-isobutyl-2-methyl-4- (4- methylphenyl) nicotinate (570 mg, yield 99%) as an oil. H-NMR (CDCl3) 6 : 0.98 (6H, d, J = 6.8 Hz), 1.39 (9H, s), 2. 17- 2.31 (1H, m), 2.39 (3H, s), 2.57 (3H, s), 2.80 (2H, d, J = 7.2 Hz), 4.13-4. 18 (2H, m), 4.23 (lui, brs), 4.40 (2H, s), 5.12 (2H, brs), 7.12 (2H, d, J = 7.7 Hz), 7.25 (2H, d, J = 7.9 Hz).

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

Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; WO2005/42488; (2005); 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

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

Adding a certain compound to certain chemical reactions, such as: 76801-93-9, name is 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide, 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 76801-93-9, SDS of cas: 76801-93-9

In a three-necked flask equipped with a stirrer and a reflux condenser, a solution of 5-amino-N, N-bis-(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzenedicarboxamide (84.6 g, 0.12 mol) N,N’-dimethyl acetamide 172ml, stirring, heating to 50 C dissolved, cooled to 10 C, add chloroacetyl chloride 62ml (88.09g, 0.78mol) dropwise for about 30 minutes, heated to 50 C stirring for 3h, cooling to 0 ~ 10 C, at 10 C, dropping 10mol / L sodium hydroxide solution 156ml, room temperature stirring 1h. After adding 100 ml of water, 59 ml of 1N hydrochloric acid was added dropwise, and the mixture was allowed to stand overnight. The filtrate was washed with water and dried to give 83.2 g of a yield of 90.0%.

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, 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Jiangsu Hengrui Medicine Co., Ltd.; Hou, Xianshan; Wang, Junyan; (11 pag.)CN106336362; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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

Application of 7681-82-5, 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 7681-82-5 as follows.

A mixture of the platinum vinylcarbene 8 (200mg, 0.261mmol) and NaI (391mg, 2.61mmol) in THF (15mL) was stirred for 5minat room temperature. All volatiles of the reaction mixture were removed under vacuum. The residue was extracted with DCM (5mL×2) and dried under reduced pressure to provide complex 14A as a yellow solid. Yield: 95% (235mg, 0.247mmol). 1H NMR (400MHz, CD2Cl2): delta 7.84 (d, J=1.8Hz, 1H, CH=CPh2) 7.63-7.68 (m, 6H), 7.38-7.49 (m, 19H), 5.04 (q, J=7.1Hz, 2H, CH2), 1.09 (t, J=7.1Hz, 3H, CH3). 31P{1H} NMR (162MHz, CD2Cl2): delta 8.6 (s, JPtP=2118.8Hz). 13C{1H} NMR (100MHz, CD2Cl2): delta 269.9 (d, J=141.3Hz, Pt=C), 154.9 (d, J=2.5Hz, HC=CPh2), 139.6 (ipso-CPh2), 138.3 (ipso-CPh2), 134.6 (d, J=10.8Hz, o- or m-PPh3), 133.5 (d, J=8.0Hz, HC=CPh2), 130.9 (d, J=50.0Hz, ipso-PPh3), 130.3, 129.6 (d, J=1.9Hz, p-PPh3), 129.2, 129.0, 128.0, 127.8, 127.2, 127.0 (d, J=9.8Hz, o- or m-PPh3), 79.2 (d, J=3.5Hz, CH2), 12.1 (CH3). Anal. Calcd. for C35H31I2OPPt: C, 44.37, H, 3.30. Found: C, 44.44, H, 3.49.

According to the analysis of related databases, 7681-82-5, the application of this compound in the production field has become more and more popular.

Reference:
Article; Ruan, Wenqing; Shi, Chuan; Sung, Herman H.Y.; Williams, Ian D.; Jia, Guochen; Journal of Organometallic Chemistry; vol. 880; (2019); p. 7 – 14;,
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. 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,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com