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. 20781-20-8, name is (2,4-Dimethoxyphenyl)methanamine, A new synthetic method of this compound is introduced below., Quality Control of (2,4-Dimethoxyphenyl)methanamine

Added to the Schlenk reaction tube 18.1 mg (0.10 mmol) copper acetate, 16.0 mg (0.025 mmol) three (2, 2′ – bipyridyl) ruthenous, 16.0 mg (0.02 mmol) tert lithium ethoxide, using Schlenk double-row tube vacuum pumping, access oxygen state, adding 79 uL (0.5 mmol) 2, 4 – dimethoxybenzylamine, 2.5 ml dimethyl sulfoxide, the use of the Schlenk tube with double row sustained and the oxygen to the reaction system, the temperature control of the reaction system 35 C, white light LED lamp (wavelength 400 – 760 nm) irradiation, stirring for 20 hours after the, adding 3 ml saturated sodium acid sulfite aqueous solution and 10 ml ethyl acetate, extraction liquid, anhydrous magnesium sulfate drying, to remove the magnesium sulfate, the resulting organic phase is concentrated, the concentrate with silica gel column chromatography, to obtain 2, 4 – dimethoxy carbonitrile, yield 90%

The synthetic route of 20781-20-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; HUAIHAI INSTITUTE OF TECH; Huaihai Technology College; TAO CHUANZHOU; Tao Chuanzhou; WANG BIN; Wang Bin; SUN LEI; Sun Lei; LIU ZHOU; Liu Zhou; ZHAI YADONG; Zhai Yadong; (5 pag.)CN107814751; (2018); A;,
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Application of 1663-61-2,Some common heterocyclic compound, 1663-61-2, name is (Triethoxymethyl)benzene, molecular formula is C13H20O3, 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: The orthoester (1.5 equiv) was added to a mixture of the 3-amino-2,2-dimethylpropionamide(1.0 equiv) in anhydrous ethanol (3 mL). Glacial acetic acid (2 equiv) was added and the reactionwas heated at reflux for 24 h. The reaction mixture was cooled and concentrated under vacuum.The product was hygroscopic and was best crystallized by adding purified chloroform and allowing itto sit under nitrogen for 4?7 days. Filtration and drying yielded the pure product.

The synthetic route of 1663-61-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Gavin, Joshua T.; Annor-Gyamfi, Joel K.; Bunce, Richard A.; Molecules; vol. 23; 11; (2018);,
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Adding a certain compound to certain chemical reactions, such as: 53087-13-1, name is 1-(Benzyloxy)-3-bromobenzene, 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 53087-13-1, Safety of 1-(Benzyloxy)-3-bromobenzene

526 mg (2.0 mmol) of 1-(benzyloxy)-3-bromobenzene, 209 mul (2.4 mmol) of morpholine, 283 mg (2.8 mmol) of sodium t-butoxide, 9 mg (0.005 mmol) of tris(dibenzylidine acetone)dipalladium (O) 19 mg (0.015 mmol) of (No.)-BINAP were placed in a flask, 5 ml of toluene was added thereto, and the mixture was stirred at 80C for 20 hours. The reaction mixture was cooled to room temperature, 20 ml of ethyl acetate was added thereto, and filtered through Cellite. The resulting filtrate was concentrated under a reduced pressure, and the residue was subjected to column chromatography using 30% ethyl acetate/hexane as an eluent to obtain 430 mg (yield 80%) of 4- (3-(benzyloxy)phenyl)morpholine.

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, 1-(Benzyloxy)-3-bromobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; KOREA RESEARCH INSTITUTE OF CHEMICAL TECHNOLOGY; OSCOTEC INC.; WO2005/123054; (2005); A1;,
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Reference of 162705-07-9, 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 162705-07-9 as follows.

General procedure: A solution of AmCA-4 (0.7mmol) in THF (5mL/mmol) was cooled at 0C and anhydrous pyridine (1.7mmol) and the corresponding phenyl chloroformate (1.0mmol) were added under inert atmosphere. The resulting mixture was stirred in the dark for 20minat 0C and for 1hat rt. After this time, H2O (3.4mL) and HCl 1M (1.7mL) were added to the reaction mixture, which was then extracted with CH2Cl2 (3¡Á20mL). The organic layer was washed with brine, and then dried on anhydrous Na2SO4. Removal of volatiles under reduced pressure afforded an oily residue which was subjected to column chromatography on silica-gel (Hexanes-EtOAc mixtures as eluant) obtaining the desired products with the yields indicated below. 6.1.2.1 53 Phenyl (Z)-(2-methoxy-5-(3,4,5-trimethoxystyryl)phenyl)carbamate (1) Off-white solid, m. p. 124-126C; 1H NMR (500MHz, CDCl3) delta 8.11 (br s, 1H), 7.52 (br s, 1H, NH), 7.39 (t, J?7.5Hz, 2H), 7.24 (t, J?7.5Hz, 1H), 7.19 (d, ?7.5Hz, 2H), 7.00 (d, J=8.5Hz, 1H), 6.76 (d, J=8.5Hz, 1H), 6.52 (s, 2H), 6.51 (d, J=12Hz, 1H), 6.45 (d, J=12Hz, 1H), 3.89 (s, 3H), 3.81 (s, 3H), 3.70 (s, 6H); 13C NMR (125MHz, CDCl3) delta (C) 152.9 (x 2), 151.3, 150.6, 146.9, 137.2, 132.7, 130.3, 126.9, (CH) 129.5, 129.3 (x 2), 129.2, 125.5, 123.9, 121.6 (x 2), 119.3, 109.6, 106.1 (x 2), (CH3) 60.8, 55.9 (x 2), 55.8; IR numax (cm-1) 3415 (N-H), 1750 (C=O); HR ESMS m/z 458.1588 [M+Na]+. Calc. for C25H25NNaO6, 458.1580.

According to the analysis of related databases, 162705-07-9, the application of this compound in the production field has become more and more popular.

Reference:
Article; Conesa-Milian, Laura; Falomir, Eva; Murga, Juan; Carda, Miguel; Meyen, Eef; Liekens, Sandra; Alberto Marco; European Journal of Medicinal Chemistry; vol. 147; (2018); p. 183 – 193;,
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Synthetic Route of 5414-19-7, These common heterocyclic compound, 5414-19-7, name is 1-Bromo-2-(2-bromoethoxy)ethane, 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.

A solution of 2-(4-phenylthiazol-2-yl)acetonitrile (0.84 g, 4.19 mmol) in THF (25 mL) was cooled to 0 C. NaH was added (0.5 g, 60% dispersion in oil) portionwise over 10 min. The resulting mixture was allowed to warm up to room temperature and stirred for 20 min. 2-Bromoethyl ether (1.58 mL, 12.5 mmol) was added dropwise. The reaction mixture was further stirred at room temperature for 1 h and then quenched with saturated NH4Cl solution. The reaction mixture was diluted with EtOAc and the organic layer was washed with H2O and brine. The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by column chromatography (silica gel 60-120 mesh, eluent 4-8% EtOAc in petroleum ether) to afford 4-(4-phenylthiazol-2-yl)tetrahydro-2H-pyran-4-carbonitrile (0.97 g, yield 85%) as a yellow solid: 1H NMR (300 MHz, CDCl3) delta 7.91-7.94 (m, 2H), 7.51 (s, 1 H), 7.37-7.48 (m, 3H), 4.07-4.14 (m, 2H), 3.87-3.96 (m, 2H), 2.32-2.43 (m, 4H). MS (ESI) m/z: Calculated for C15H14N2OS: 270.08; found: 271.2 (M+H)+.

The synthetic route of 5414-19-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Tempero Pharmaceuticals, Inc.; BALOGLU, Erkan; GHOSH, Shomir; LOBERA, Mercedes; SCHMIDT, Darby; EP2533783; (2015); B1;,
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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. 20781-20-8, name is (2,4-Dimethoxyphenyl)methanamine, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C9H13NO2

To a solution of 5-fluoro-2-nitrobenzoic acid (6.6g, 35.66 mmol) in dichloromethane (100 mL) were added DIPEA (9.22 g, 71.3 mmol), HOBt (6.0 g, 39.2 mmol) and EDCI (10.2 g, 53.5 mmol). After about 15 min stirring, to the reaction mixture was added a solution of 2,4-dimethoxybenzyl amine (5.96 g, 35.66 mmol) in dichloromethane (50 mL) dropwise under nitrogen atmosphere. The resulting mixture was stirred under nitrogen atmosphere at room temperature for 16 h. The reaction mixture was washed successively with 1N HC1 (100 mL), sat. NaHCCb (100 mL) and brine (100 mL). The organic phase was then dried over MgS04. Filtration and solvent removal in vacuo afforded a yellowish solid, wt: 9.3g (78%). MS: [M+l] = 335.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 20781-20-8.

Reference:
Patent; AGENEBIO, INC.; MEKONNEN, Belew; BUTERA, John, A.; HUANG, Jianxing; PATEL, Hemantbhai; JIANG, Qin; HERR, Robert, Jason; MAYHEW, Nicholas, James; FREEMAN, Emily, Elizabeth; (682 pag.)WO2019/246300; (2019); A1;,
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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. 4698-11-7, name is 10-Methoxy-5H-dibenzo[b,f]azepine, A new synthetic method of this compound is introduced below., Formula: C15H13NO

10-Methoxy-5H-dibenzo[b,f]azepine 4 (500 g, 2.23 mol) and isopropanol (1.0 L) were charged into a round bottomed flask and stirred for 5-10 min. 50% Aqueous hydrochloride solution (250 mL) was then added slowly to the mixture at 25-35 ?C and stirred for 15 min. The reaction mixture was heated to 60-65 ?C and maintained for 2-3 h. The progress of the reaction was monitored by TLC, and after completion of the reaction (by TLC), ethyl acetate (1.5 L) and water (1.0 L) were added into the reaction mixture and stirred for 5-10 min. Organic layer was separated and the aqueous layer was extracted with ethyl acetate (1.5 L). The combined organic layer was washed with 5% caustic lye solution (500 mL) followed by 10 % NaCl solution (500 mL) and evaporated at 50-55?C under reduced pressure. n-Hexane (500 mL) was then added into the crude product at 25-30 ?C and stirred for 1-2 h. The obtained solid was collected by filtration, washed with n-hexane (250 mL) and dried at 60-65 ?C to afford the title compound 6 as yellow solid (400 g) in 85.4% yield and >98.2% purity. Spectroscopic data were found to be in agreement with the data collected from authentic sample of intermediate 6. IR (KBR): 3329, 3284, 3040, 1643, 1474, 1309, 753 cm-1; 1H NMR (400 MHz, CDCl3): delta 3.72 (2H, s), 6.78-7.91 (8H, m); 13C NMR (400 MHz, CDCl3): delta 49.4, 119.1, 119.2, 119.8, 124.1, 124.5, 127.7, 127.9, 129.8, 130.3, 133.7, 141.5, 146.8, 190.1; HRMS calcd for C14H11NO, 210.0919; found 210.0909.

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; Ravinder; Rajeshwar Reddy; Sridhar; Murali Mohan; Srinivas, Katkam; Panasa Reddy; Bandichhor, Rakeshwar; Tetrahedron Letters; vol. 54; 22; (2013); p. 2841 – 2844;,
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Synthetic Route of 29026-74-2, 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. 29026-74-2, name is 2-Isopropoxyaniline belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Step 2; preparation of 2-[(2-Hydroxy-ethyl)-(2-isopropoxy-phenyl)-amino]-ethanol; 2-Isopropoxy-phenylamine (5 gm, 0.033 mole) was dissolved in chlorobonzene (25 ml) and to reaction mixture was added triethylamine (16.7 gm, 0.165 mole) under stirring. After this, 2-chloroethanol (13.25 gm, 0.165 mole) was added and reaction mixture refluxed for 12 to 15 hours. The reaction was quenched by adding water (50 ml) to it and extracted with dichloromethane (3×50 ml). The organic layer dried over anhydrous sodium sulphate (Na2S04) and concentrated to give the crude product. The crude product thus obtained was purified on a silica gel (60-120 mesh) column using dichloromethane-methanol as eluent. Yield: 5.8 gm (73%)

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

Reference:
Patent; RANBAXY LABORATORIES LIMITED; WO2005/113498; (2005); A1;,
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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. 1978-39-8, name is 5-Fluoro-2-methoxyaniline belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 5-Fluoro-2-methoxyaniline

To a solution of compound Al (400 rng, 0.53 mrnoi) and 5-fluoro-2-rnethoxyaniline (150,7mg, 1.07 mmoi) intoluene (10 rnL) was added Ti(O-i] r)4 (151.6 mg, 0.53 mmoi). Themixture was stirred at 120 C over night under N2. The mixture was quenched with [120 (50 rnL) and extracted with DCM (20 mL x 3). The combined organic layer was dried over potassium carbonate, filtered and concentrated. The residue was purified by silica gel column chromatography (DCMMeOH = 15/i) to afford the crude products 29-1 and 29-2 (320 mg) as a yellow solid. LC-MS: m/z 89.4 [M+I-[.

The synthetic route of 1978-39-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AGRIMETIS, LLC; CALABRESE, Andrew; (110 pag.)WO2018/132288; (2018); A1;,
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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. 103-50-4, name is Benzyl ether, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C14H14O

General procedure: To a sealed tube containing the respective azobenzene 1 (0.25 mmol), dibenzyl ether 2 (0.75 mmol), Pd(OAc)2 (0.025 mmol), and DCE/AcOH (1:1, v/v, 1 mL in all) was added TBHP (1.5 mmol). After stirring vigorously at 60 C for 12 h, the mixture was evaporated under vacuum. The corresponding product 3 was isolated by silica gel column chromatography with a PE/EtOAc mixture as eluent.

According to the analysis of related databases, 103-50-4, the application of this compound in the production field has become more and more popular.

Reference:
Article; Hong, Gang; Aruma, Alfred Njasotapher; Zhu, Xiaoyan; Wu, Shengying; Wang, Limin; Synthesis; vol. 48; 8; (2016); p. 1147 – 1158;,
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