Tag: M.W=200-300

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 444-29-1 as follows. COA of Formula: C7H4F3I

General procedure: A solution of Ar3In or (RC?C)3In (0.37mmol, ca. 0.18M in dry THF) was added to a mixture of MCM-41-N,N-Pd(0) (25mg, 1molpercent) and aryl iodide (1mmol) in dry THF (2mL) under Ar. The resulting mixture was refluxed under Ar until the starting material had been consumed (TLC). After being cooled to room temperature, the mixture was diluted with Et2O (30mL) and filtered. The palladium catalyst was washed with DMF (2×5mL), Et2O (2×5mL) and reused in the next run. The filtrate was washed with sat. aq NaHCO3 (5mL), water (3×10mL) and dried over MgSO4, filtered, and concentrated under vacuum. The residue was purified by flash chromatography on silica gel to give the desired cross-coupling product.

According to the analysis of related databases, 444-29-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Lei, Zhiwei; Liu, Haiyi; Cai, Mingzhong; Journal of Organometallic Chemistry; vol. 852; (2017); p. 54 – 63;,
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Electric Literature of 19099-54-8, 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 19099-54-8 as follows.

General procedure: A dried round-bottomed flask was charged with aryl iodide (0.30 mmol, 1.0 equiv), ortho-bromobenzoyl chlorides (0.36 mmol, 1.2 equiv), norbornadiene (0.60 mmol, 2.0 equiv), Pd(OAc)2 (5 mol %), triphenylphosphine (12.5 mol %), Cs2CO3 (0.675 mmol, 2.25 equiv), and DMF (4 mL). The mixture was stirred at 105 C under nitrogen atmosphere for 10 h. After cooling to room temperature, the mixture was diluted with ethyl acetate (5 mL) and brine (10 mL), and extracted with ethyl acetate (3 × 10 mL). The combined organic phase was washed with brine, dried with anhydrous Na2SO4, filtered, and concentrated under reduced pressure. The crude product was purified by column chromatography on silica gel (petroleum ether/ethyl acetate as eluent) to afford the target compounds

According to the analysis of related databases, 19099-54-8, the application of this compound in the production field has become more and more popular.

Reference:
Article; Zhong, Yue; Wu, Wen-Yu; Yu, Shao-Peng; Fan, Tian-Yuan; Yu, Hai-Tao; Li, Nian-Guang; Shi, Zhi-Hao; Tang, Yu-Ping; Duan, Jin-Ao; Beilstein Journal of Organic Chemistry; vol. 15; (2019); p. 291 – 298;,
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Synthetic Route of 335349-57-0, These common heterocyclic compound, 335349-57-0, name is 5-Chloro-4-iodo-2-nitroaniline, 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.

Example B4 [4-Iodo-2-nitro-5-(2,2,2-trifluoro-ethoxy)-phenyl]-carbamic acid tert.-butyl ester The title compound was prepared via the di-Boc-compound from 4-iodo-2-nitro-5-(2,2,2-trifluoro-ethoxy)-phenylamine [prepared by stirring 5-chloro-4-iodo-2-nitro-phenylamine (Example A1) (8.95 g, 30 mmol), 2,2,2-trifluoroethanol (30 mL) and KOH (4.36 g, 66 mmol) in DMSO (60 mL) at 23 C. for 35 days.] (10.41 g, 29 mmol) and Boc2O (12.87 g, 59 mmol), followed by treatment with 2 eq. TFA in CH2Cl2 according to the general procedure B (method c). Obtained as a yellow solid (13.34 g, 100%). MS (ISN) 461 [(M-H)-].

Statistics shows that 5-Chloro-4-iodo-2-nitroaniline is playing an increasingly important role. we look forward to future research findings about 335349-57-0.

Reference:
Patent; Hoffman-La Roche Inc.; US6544985; (2003); B2;,
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 1450754-38-7 as follows. Product Details of 1450754-38-7

To a mixture of 3-(but-3-yn-1-yl)-3-(2-iodoethyl)-3H-diazirine (70 mg, 282 imol, 1 eq) and 3- hydroxybenzaldehyde (34.5 mg, 282 imol, 1 eq) in 1 mL of DMF was added Cs2CO3 (276 mg, 847 imol, 3 eq) in one portion at 15C under N2. The mixture was stirred at 60 C for 12 hours.The reaction mixture was diluted with 3 mL of H20 and extracted three times with 9 mL of EtOAc. The combined organic layers were washed twice with 6 mL of brine, dried over Na2SO4, filtered and concentrated under reduced pressure to give a residue. The residue was purified by prep-TLC (Si02, eluting with petroleum ether: ethyl acetate = 3:1) to give 40 mg of crude A-2 as colorless oil.

According to the analysis of related databases, 1450754-38-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; AQUINNAH PHARMACEUTICALS, INC.; BURNETT, Duane, A.; VACCA, Joseph, P.; (310 pag.)WO2018/119395; (2018); A1;,
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14452-30-3, name is 1-(3-Iodophenyl)ethanone, 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. Formula: C8H7IO

General procedure: Aryl halide (1.1 eq.), Au complex 1 (1.0 eq.) and a palladium catalyst (10 mol%) was dissolved in THF under nitrogen. The mixture was refluxed until the starting Au-complex was consumed (monitored by TLC). The reaction mixture was concentrated under reduced pressure. The residue was separated and purified by chromatography, to afford the corresponding cross-coupling product.

The synthetic route of 14452-30-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Tanimoto, Ryu; Suzuki, Shuichi; Kozaki, Masatoshi; Okada, Keiji; Chemistry Letters; vol. 43; 5; (2014); p. 678 – 680;,
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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. 10297-05-9, name is 1-Chloro-4-iodobutane, A new synthetic method of this compound is introduced below., name: 1-Chloro-4-iodobutane

817 mg (4.041 mmol) of 5-hydroxypsoralen and 1.413 g (6.47 mmol) of 4-chlorobutyl iodide were refluxed in 80 ml of acetone in the presence of an excess of (3.0 g) anhydrous potassium carbonate for 30 hours. The progress of the reaction was monitored by thin layer chromatography. After 30 hours the reaction mixture was concentrated under reduced pressure and distilled off the solvent almost completely. The oily residue was cooled and diluted with water. The aqueous solution was then acidified with concentrated hydrochloric acid to pH 1. The slurry was stirred for 15-20 min and extracted with 3.x.100 ml of dichloromethane. The dichloromethane layer was extracted with 1.x.25 ml of 1percent sodium hydroxide to separate trace amounts of un-reacted 5-hydroxypsoralen. The dichloromethane layer was washed with 30 ml of 2percent hydrochloric acid and further washed with water to neutral pH. The dichloromethane layer was dried over anhydrous sodium sulfate and concentrated to dryness. The resulting residue was then suspended in petroleum ether and filtered to wash out the excess 4-chlorobutyl iodide. The resulting 5-(4-chlorobutoxy)psoralen was used for the synthesis of various derivatives without further purification. Yield: 1.10 g (92.98percent) Melting point: 115.4-115.6° C. 1H-NMR (500 MHz, CDCl3): delta [ppm]=8.15 (d, 1H, 3J=9.75 Hz, 3-H), 7.60 (d, 1H, 3J=2.62 Hz, 2′-H), 7.17(s, 1H, 8-H), 6.95 (d, 1H, 3J=2.15 Hz, 3′-H), 6.29 (d, 1H, 3J=9.79 Hz, 4-H), 4.52 (t, 2H, 3J=5.44 Hz, 5-OCH2CH2CH2CH2Cl), 3.68 (t, 2H, 3J=5.89 Hz, 5-OCH2CH2CH2CH2Cl), 2.08 (p, 4H, 3J=3.06 Hz, 5-OCH2CH2CH2CH2Cl).; 500 mg (2.473 mmol) of 5-hydroxypsoralen and 893 mg (4.088 mmol) of 4-iodo-1-chlorobutane were stirred at 25° C. in 30 ml of anhydrous acetone in the presence of an excess (2.0 g) of anhydrous potassium carbonate for 28 hours. The progress of the reaction was monitored by thin layer chromatography. After 28 hours the reaction mixture was concentrated under reduced pressure and distilled off the solvent almost completely. The oily residue was cooled and diluted with water. The aqueous solution was then acidified with concentrated hydrochloric acid to pH 1. The slurry was stirred for 15-20 min and filtered. The solids were washed with water to neutral pH and dried. The dried solids were suspended in petroleum ether, filtered and dried under vacuum.

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; The Regents of the University of California; US2006/79535; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 52807-27-9, These common heterocyclic compound, 52807-27-9, name is 4-Chloro-2-iodoanisole, 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: A mixture of the aryl halide (0.6 mmol), arylboronic acid (2.5 equiv), Mo(CO)6 (1.5 equiv), DIPEA (3.0 equiv), palladacycle 1 (1 mol % Pd), and water (1.0 mL) was heated in a pressure tube at 140 C under microwave irradiation. The reaction was monitored by TLC. When the reaction has completed, the reaction mixturewas cooled to room temperature, poured into EtOAc (20 mL) and washed successively with water (310 mL). The organic layer was dried over anhydrous MgSO4, filtered and concentrated. The crude product was then purified by column chromatography to give pure 4.

The synthetic route of 52807-27-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Ang, Wei Jie; Lo, Lee-Chiang; Lam, Yulin; Tetrahedron; vol. 70; 45; (2014); p. 8545 – 8558;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 618-91-7,Some common heterocyclic compound, 618-91-7, name is Methyl 3-iodobenzoate, molecular formula is C8H7IO2, 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.

3-((E)-2-benzyloxycarbonyl-2-tert-butoxycarbonylamino- vinyl)-benzoic acid methyl ester: To 84A (10 g, 0.036 mol) dissolved in DMF (100 mL) were added methyl 3-iodobenzoate (9.5 g, 0.036 mol), palladium acetate (0.25 g, 1.08 mmol), tetrabutylammonium chloride (H g, 0.039 mol), and triethyl amine (15 mL, 0.108 mol). The mixture was flushed with nitrogen for 1 h, then heated at 85 0C overnight. The reaction mixture was diluted with brine and extracted with ethyl acetate. The organic layer was washed with brine and concentrated. The crude product was purified by flash chromatography on silica gel eluting with 10% ethyl acetate in petroleum ether to give 84B (10 g, 67.5%).

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

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; WO2007/70826; (2007); 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 608-28-6 as follows. Recommanded Product: 2-Iodo-1,3-dimethylbenzene

General procedure: The aryl iodide (1.0 mmol), boronic acid (2.0 mmol), PEPPSI-IPr (0.03 mmol), and Cs2CO3 (2.5 mmol) were placed into a 10 mL glass sleeve fitted with a rubber septum. The sleeve was then evacuated and backfilled with CO(g) three times. Dioxane (5.0 mL) was added, and the mixture was sparged with CO(g) for 2 min. The rubber septum was then removed, and the glass sleeve was quickly sealed in a stainless steel pressure reactor. The reactor was evacuated and backfilled with CO(g) (three cycles, 60 psi). The reactor was heated at 140 C (oil bath) with stirring for 24 h at 60 psi of CO(g). The reaction mixture was filtered through a pad of Celite, washing with EtOAc. The filtrate was washed with H2O (20 mL), brine (20 mL), dried (MgSO4), filtered, and concentrated under reduced pressure. The crude residue was purified by flash column chromatography, eluting with the indicated solvent to afford the product benzophenone.

According to the analysis of related databases, 608-28-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; O’Keefe, B. Michael; Simmons, Nicholas; Martin, Stephen F.; Tetrahedron; vol. 67; 24; (2011); p. 4344 – 4351;,
Iodide – Wikipedia,
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Reference of 5460-32-2, 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. 5460-32-2 name is 4-Iodo-1,2-dimethoxybenzene, 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.

4-Iodoveratrole (26.0 g, 0.0985M) in acetic acid (25 ml) was treated with bromine (6.5 ml, 0.127M) in acetic acid (30 ml) and stirred at room temperature for one hour. The mixture was diluted with water (300 ml) and treated with sodium bisulfite to discharge the excess bromine. The white solid was filtered, washed with water and dried in vacuo over P2 O5 to give 4-bromo-5-iodoveratrole (33.0 g, 95percent yield) as a white solid, mp 98°-100° C. (literature: Baker et al., J. Chem. Soc. 3986 (1961), mp 102°-104° C.). NMR (CDCl3) delta 3.83 ppm (s, 6H, (2x) OCH3), 7.06 (s, 1H, ArH), 7.21 (s, 1H, ArH).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Iodo-1,2-dimethoxybenzene, and friends who are interested can also refer to it.

Reference:
Patent; Ortho Pharmaceutical Corporation; US4761413; (1988); A;,
Iodide – Wikipedia,
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