Author: Jessica.F

Adding a certain compound to certain chemical reactions, such as: 2062-98-8, name is Perfluoro(2-methyl-3-oxahexanoyl) fluoride, belongs to ethers-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 2062-98-8, COA of Formula: C6F12O2

While the solution containing compound (c1-1) was stirred at 0C, 1.7 g of triethylamine was added. Then, 4.4g of 2-(heptafluoropropoxy)-2,3,3,3-tetrafluoropropionic acid fluoride (compound d1-1) was dropwise added. After completionof dropwise addition, the solution was stirred at room temperature for 1 hour to obtain a solution containingcompound (m1-1). The solution containing compound (m1-1) was poured into ice water, followed by extraction three times withethyl acetate. Then, the resulting organic layer was dried over magnesium sulfate to remove the solvent, and the residuewas purified by silica gel column chromatography (eluent: ethyl acetate/hexane=1/2 (volume ratio)) to obtain 2.0 g ofcompound (m1-1). Compound (m1-1) was identified by 1H-NMR and 19F-NMR. NMR spectra of compound (m1-1): 1H-NMR (300.4MHz, solvent:CDCl3, standard:TMS) delta (ppm): 1.85(s, 6H), 4.27(t, J=4.8, 2H), 4.52(t, J=4.8, 2H),5.87(dd, J=10.5, 10.8, 1 H), 6.16(dd, J=10.5, 17.1, 1H), 6.45(dd, J=17.1, 17.4, 1H), 6.92(d, J=9.0, 2H), 7.90(d,J=9.0, 2H). 19F-NMR(282.7MHz, solvent:CDCl3, standard:CFCl3)delta5(ppm):-132.0(m, 1F), – 129.6(m, 2F), -85.4(m, 1F), -81.2(m, 6F), -79.5(m, 1F).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Perfluoro(2-methyl-3-oxahexanoyl) fluoride, and friends who are interested can also refer to it.

Reference:
Patent; Asahi Glass Company, Limited; ITO, Masahiro; TSURUOKA, Kaori; EP2792665; (2014); A1;,
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Synthetic Route of 592-55-2, These common heterocyclic compound, 592-55-2, name is 1-Bromo-2-ethoxyethane, 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 2: 4- {3-Hydroxy-3- [4- (2-ethoxyethoxy)-5, 5, 8, 8- tetramethyl-5,6, 7, 8-tetrahydronaphth-2-yl] prop-1-ynyl}- benzoic acid; a. 5,5, 8, 8-Tetramethyl-4- (2-ethoxyethoxy)- 5,6, 7,8-tetrahydronaphthalene-2-carbaldehyde 36 g (156 mmol) of 4-hydroxy-5,5, 8,8-tetra- methyl-5,6, 7, 8-tetrahydronaphthalene-2-carbaldehyde are dissolved in 400 mL of anhydrous DMF. 6.5 g (163 mmol) of 60% sodium hydride are added portionwise and the reaction medium is stirred for 1 hour. 25 g (163 mmol) of 2-ethoxyethyl bromide are added portionwise and the medium is stirred at room temperature for 2 hours and then hydrolysed and extracted with ethyl ether. The organic phase is washed with 1N sodium hydroxide solution, and then three times with water. The residue obtained is purified by chromatography (eluent: heptane). A yellow oil is obtained (m = 40.7 g; yield = 86%).

The synthetic route of 592-55-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GALDERMA RESEARCH & DEVELOPMENT, S.N.C.; WO2005/56510; (2005); A2;,
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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. 7025-06-1, name is 1-Bromo-2-phenoxybenzene, A new synthetic method of this compound is introduced below., Formula: C12H9BrO

The THF solution (50 mL) of the compound 3 (g [ 7.5 ], 40mmol) was dropped at the roomtemperature at metal magnesium (1 g, 40mmol), 1,2dibromoethane (0.2 mL), and themixture of THF (50 mL), and was stirred into them for 3 hours. The THF solution (20 mL) ofthe phosphorus trichloride (2.6 mL, 30mmol) was dropped here at 78 degree C, and it stirredat the room temperature for 1 hour. It removed under decompression of a solvent and anexcessive phosphorus trichloride, THF (50 mL) was newly added, and the solution of thecompound 4 was obtained. The solution of the compound 2 of the preceding paragraph wasdropped here at 78 degree C, and it stirred at the room temperature for 2 hours to make the solution of the compound 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; JAPAN POLYETHYLENE CORPORATION; JAPAN POLYPROPYLENE CORPORATION; XIN, SHIXUAN; SHIMIZU, FUMIHIKO; SATO, NAOMASA; TANNA, AKIO; (45 pag.)JP5812764; (2015); B2;,
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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. 1663-61-2, name is (Triethoxymethyl)benzene, A new synthetic method of this compound is introduced below., Recommanded Product: (Triethoxymethyl)benzene

1,1,1-Trimethoxyethane (35 mg, 0.291 mmol) and 3 mgcamphorsulfonic acid (0.012 mmol) were added to asolution of 113 mg heptoside 1 (0.242 mmol) in 1 cm3dry CH2Cl2 and stirred for 1 h at rt when TLC showed fullconversion of 1 into intermediate 11 (Rf = 0.33, hexane/EtOAc = 2/1).

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:
Article; Walter, Martin; Kohout, Claudia; Blaukopf, Markus; Kosma, Paul; Monatshefte fur Chemie; vol. 148; 1; (2017); p. 111 – 119;,
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Related Products of 112970-44-2, 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 112970-44-2 as follows.

Step 2. Synthesis of N-(2-bromo-3-methoxyphenyl)-2,2,2-trifluoroacetamide (C24) Trifluoroacetic anhydride (3.0 mL, 22 mmol) was added to a solution of 2-bromo-3-methoxyaniline (C23) (2.57 g, 10.77 mmol) and triethylamine (4.51 mL, 32.3 mmol) in dichloromethane (30 mL) at -78 C. The reaction was allowed to warm to room temperature and stirring was continued for 18 hours, whereupon the mixture was poured into water (40 mL) and extracted with dichloromethane (2*20 mL). The combined organic layers were dried over sodium sulfate and concentrated in vacuo. Purification via silica gel chromatography (Gradient: 0% to 30% methyl tert-butyl ether in hexanes) afforded the title compound as a colorless solid. Yield: 2.97 g, 9.96 mmol, 92%. GCMS m/z 297, 299 (M+). 1H NMR (400 MHz, CDCl3) delta 3.94 (s, 3H), 6.81 (dd, J=8.4, 1.2 Hz, 1H), 7.35 (dd, J=8.4, 8.3 Hz, 1H), 7.97 (dd, J=8.3, 1.3 Hz, 1H), 8.59 (br s, 1H).

According to the analysis of related databases, 112970-44-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Pettersson, Martin Youngjin; Johnson, Douglas Scott; Subramanyam, Chakrapani; O’Donnell, Christopher John; Ende, Christopher William Am; Fish, Benjamin Adam; Green, Michael Eric; Mullins, Patrick Bradley; Stiff, Cory Michael; Tran, Tuan Phong; Navaratnam, Thayalan; US2012/252758; (2012); A1;,
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Synthetic Route of 175278-09-8,Some common heterocyclic compound, 175278-09-8, name is 4-Bromo-2-(trifluoromethoxy)aniline, molecular formula is C7H5BrF3NO, 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: Triphosgene (0.14 g, 0.48 mmol) was dissolved in anhydrous CH2Cl2 (15 mL) and the mixture was stirred on the ice-bath for 15 min. 3-Bromo-5-(trifluoromethyl)aniline (0.3 g, 1.2 mmol) in anhydrous CH2Cl2 (10 mL) was added dropwise to the above mixture and stirring continued for 20 min. Et3N (0.2 mL, 1.44 mmol) diluted with CH2Cl2 (5 mL) was then added into the mixture. Stirring was continued for 20 min and a solution of Et3N (0.2 mL, 1.44 mmol), 4-pyridin-3-ylaniline (5) (0.2 g, 1.2 mmol) in anhydrous CH2Cl2 (20 mL) was added. After completion of the action, the reaction was quenched with dilute Na2CO3. The organic layer was washed with water and brine, and dried over Na2SO4. After filtration and concentration in vacuo, the residues was purified by silica gel flash chromatography (PE/AcOEt = 6:1) yielding (L1). yield 73%

The synthetic route of 175278-09-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Su, Ping; Wang, Jinfeng; Shi, Yaling; Pan, Xiaoyan; Shao, Ruili; Zhang, Jie; Bioorganic and Medicinal Chemistry; vol. 23; 13; (2015); p. 3228 – 3236;,
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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. 261762-35-0, name is 5-Bromo-1,2-difluoro-3-methoxybenzene belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C7H5BrF2O

The title compound was prepared by reaction of 5-bromo-1,2-difluoro-3-methoxybenzene (1.03 g, 4.62 mmol, 1.0 equiv) andmagnesium (112 mg, 4.61 mmol, 1.0 equiv) and iodine (~2 mg) in13 ml diethylether under reflux for 2 h. Carbon dioxidewas bubbledthrough the solution at 10 C until all solvent (13 ml) was evaporatedtwo times. The crude product was dissolved in 10ml THF andcarbon dioxidewas bubbled through the solution for additional 1 h.The reaction was quenched with 1M HCl, extracted with ethyl acetate,dried with magnesium sulfate and concentrated underreduced pressure to afford the crude product, which was purifiedby flash chromatography; yield: 31% (265 mg). 1H NMR (300 MHz,MeOH-d4) d 7.65e7.45 (m, 2H), 3.99 (s, 3H).

The synthetic route of 261762-35-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Abdelsamie, Ahmed S.; Salah, Mohamed; Siebenbuerger, Lorenz; Hamed, Mostafa M.; Boerger, Carsten; van Koppen, Chris J.; Frotscher, Martin; Hartmann, Rolf W.; European Journal of Medicinal Chemistry; vol. 178; (2019); p. 93 – 107;,
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Application of 74137-36-3, 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. 74137-36-3, name is 1,3-Dibromo-5-methoxybenzene belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A THF ( 150 mL) solution containing l ,3-dibromo-5-methoxybenzene (1.10 g, 4.10 mmol) and Pd(PPh3)4 (0.48 g, 0.41 mmol) was charged with a 0.5 M THF solution of 2-pyridylzinc bromide (21 mL, 10 mmol). The solution was stirred at reflux for 14 h, cooled and then quenched with a saturated aqueous NaHCO, solution ( 100 mL) and washed with aqueous EDTA. The crude product was extracted with diethyl ether (2 x 100 mL), and the organic fractions were collected and dried over MgS04. The solvent was removed in vacuo to afford an oil that was purified by column chromatography [AI2O3: Epsiloniota20, Rf = 0.60]; the resultant oily product converted to a white solid upon standing (850 mg; yield = 78percent). NMR (300 MHz, CDC13): delta = 8.70 (d, 2H, 3 J = 7 Hz, Ha), 8.20 (s, 1H, Hf, 7.77 (d, 2H, 3 J = 8 Hz, Hf, 7.75 (t, 2H, 3 J = 8 Hz, Hf), 7.66 (s, 2H, He), 7.25 (t, 2H, 3 J = 8 Hz, Hh), 3.97 (s, 3H, Hg); 13C NMR (100 MHz, CDCI3): delta = 160.7, 157.2, 149.7, 141.4, 136.9, 122.5, 121.0, 1 18.2, 1 13.3, 55.8; HRMS (EI): mlz, = 262.1 101 [(M)+] (calcd for Ci7Hi4N20+: mlz = 262.1 106).

The synthetic route of 1,3-Dibromo-5-methoxybenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BERLINGUETTE, Curtis P.; KOIVISTO, Bryan; ROBSON, Kiyoshi; WO2011/32269; (2011); A1;,
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Application of 262587-05-3, These common heterocyclic compound, 262587-05-3, name is 1-Bromo-3-(difluoromethoxy)benzene, 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 1; Preparation of 2-nitro-5- (3-difluoromethoxyphenylthio) – p-xylene [nitroderivative of formula (III) ]; 4.36 g (0.109 moles) of sodium hydride are sus¬ pended in 80 ml of N, N-dimethylformamide at 0C. 20 g of 4-nitro-2 , 5-dimethylthiophenol (0.109 moles) dis¬ solved in 67 ml of N, N-dimethylformamide are added dropwise under stirring. 24.4 g of l-bromo-3- (difluoromethoxy) benzene (0.109 moles) dissolved in 20 ml of N, N-dimethylformamide are then added dropwise; catalytic Cu and CuCl are subsequently added and the reaction temperature is brought to 150 C for 1 h.After GC control, the reaction mixture is cooled to room temperature, filtered on a celite bed, diluted with water and extracted with ethyl acetate. The or¬ ganic phase is anhydrified with sodium sulfate, and then filtered and evaporated.The product thus obtained is purified on silica gel eluting with hexane/ethyl acetate 9:1. 30 g of the desired product are obtained. GC-MS : M+ = 325

Statistics shows that 1-Bromo-3-(difluoromethoxy)benzene is playing an increasingly important role. we look forward to future research findings about 262587-05-3.

Reference:
Patent; ISAGRO RICERCA S.R.L.; GUSMEROLI, Marilena; FILIPPINI, Lucio; PELLACINI, Franco; BRAVINI, Paolo; ELMINI, Alexia; VAZZOLA, Matteo Santino; BADARACCO, Christian; WO2012/25450; (2012); A1;,
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Electric Literature of 6346-09-4, 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. 6346-09-4 name is 4,4-Diethoxybutan-1-amine, 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.

To a mixture of 4.2 g (20 mmol) of 4-chlorobenzenesulfonyl chloride and 2.5 mL oftrimethylamine in 100 mL of dichloromethane at cooling (5-8 C) was added 3.2 g (20 mmol) of 4,4-diethoxybutan-1-amine. The reaction mixture was stirred at room temperature for 12 h, washed with saturated solution of NaHCO3 (100 mL), the organic layer was separated and evaporated in a vacuum. Yield 5.4 g (93%). 1H NMR spectrum (CDCl3), , ppm: 1.12t (3H, CH3, J 7.0 Hz), 1.38-1.48 m (1H, CH2), 1.69-1.77 m (1H, CH2), 1.81-1.87 m (1H, CH2), 1.91-2.09m (1H, CH2), 3.07-3.15 m (1H, CH2), 3.30-3.39 m(1H, CH2), 3.42-3.50 m (1H, CH2), 3.66-3.72 m (1H, CH2), 5.15-5.19 m (1H, CH), 7.43 d (2H arom, J 8.5 Hz), 7.75 d (2H arom, J 8.5 Hz). 13C NMR spectrum (CDCl3), ppm: 14.98, 14.99, 23.12, 32.76, 47.22, 63.17,90.21, 128.84, 129.25, 137.73, 139.01.

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

Reference:
Article; Smolobochkin; Anikina; Gazizov; Burilov; Pudovik; Russian Journal of Organic Chemistry; vol. 53; 2; (2017); p. 199 – 202; Zh. Org. Khim.; vol. 53; 2; (2017); p. 209 – 212;,
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