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. 1758-46-9, name is 2-Phenoxyethylamine, A new synthetic method of this compound is introduced below., SDS of cas: 1758-46-9

General procedure: Et3N (4.3 mmol) and 97% EtOCOCl (4.3 mmol) in dry CHCl3(25 mL) were added to a solution of the suitable carboxylic acid 24a,24b or 25 (4.3 mmol) at 0 C. After 30 min at 0 C under stirring asolution of the suitable amine (2-phenoxyethanamine, 2-(2-methoxyphenoxy)ethanamine [37], 2-(2,6-dimethoxyphenoxy)ethanamine [38], or 1-(2-methoxyphenyl)piperazine) (4.3 mmol)in dry CHCl3 (10 mL) was added and the reaction mixture was left atroom temperature for 3 h. The solution was washed with 2 N HCl and 2 N NaOH. The organic layer was dried over Na2SO4. After evaporation of the solvent the residue was purified by column chromatography eluting with cyclohexane/EtOAc (7:3).

The synthetic route of 1758-46-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Del Bello, Fabio; Bonifazi, Alessandro; Giorgioni, Gianfabio; Quaglia, Wilma; Amantini, Consuelo; Morelli, Maria Beatrice; Santoni, Giorgio; Battiti, Francisco O.; Vistoli, Giulio; Cilia, Antonio; Piergentili, Alessandro; European Journal of Medicinal Chemistry; vol. 168; (2019); p. 461 – 473;,
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Reference of 2688-84-8, A common heterocyclic compound, 2688-84-8, name is 2-Phenoxyaniline, molecular formula is C12H11NO, 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.

2-Phenoxyaniline (0.185 g, 1.0 mmol), 6-chloropyrazine-2-carboxylic acid (0.158 g, 1.0 mmol) and 30 mL of dichloromethane were added to the reaction flask, and Et3N (0.202 g, 2.0 mmol) was added. Then, EDCI (0.287 mg, 1.5 mmol), HOBt (0.20 g, 1.5 mmol) was added, and the reaction was carried out at 25 C for 2.5 hours. The reaction was completed by TLC, and the reaction was completed. The reaction mixture was washed twice with water and once with saturated brine. The organic phase is dried over anhydrous sodium sulfate, de-solued to give a crude product, and recrystallized from ethanol.Brick red solid, m.p. 138-140 C, yield 79.0%

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; Chen Lei; (6 pag.)CN108997228; (2018); A;,
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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. 162705-07-9, name is (Z)-2-Methoxy-5-(3,4,5-trimethoxystyryl)aniline, A new synthetic method of this compound is introduced below., Recommanded Product: (Z)-2-Methoxy-5-(3,4,5-trimethoxystyryl)aniline

General procedure: To a solution of substituted benzyl-1H-1,2,3-triazole-4-carboxylic acids (18a-e, 1 mmol) in dry dimethylformamide, EDCI (1.2 mmol) and HOBT (1.2 mmol) were added and the reaction mixture was stirred for 20 min. To the reaction mixture, amino Z-stilbenes (16, 17, 1 mmol) was added and stirred at room temperature for 12 h. The solvent was removed and the residue was dissolved in dichloromethane (50 mL), washed with 5% HCl (2 20 mL), 5% NaHCO3 (2 20 mL), and brine solution (20 mL). The organic layer was separated, dried over anhydrous Na2SO4, filtered, and the solvent was removed to give a crude product which was purified by chromatography (ethyl acetate/hexanes) to givethe desired product (6a-e, 7a-e).

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; Kamal, Ahmed; Shaik, Bajee; Nayak, V. Lakshma; Nagaraju, Burri; Kapure, Jeevak Sopanrao; Shaheer Malik; Shaik, Thokhir Basha; Prasad; Bioorganic and Medicinal Chemistry; vol. 22; 19; (2014); p. 5155 – 5167;,
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Some common heterocyclic compound, 1535-75-7, name is 2-(Trifluoromethoxy)aniline, molecular formula is C7H6F3NO, 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. SDS of cas: 1535-75-7

Synthesis Example 32 Synthesis of 2-Trifluoromethoxybenzenesulfonamide [Compound (III-12)] Using 2-trifluoromethoxyaniline [Compound (XXV-12)] (5 g, 0.0282 mmol), 7.3 g (percent yield: 99.4%) of 2-trifluoromethoxybenzenesulfonyl chloride [Compound (XXII-12)] was synthesised according to the process of Synthesis Example 31 (3). Thereafter, the compound (III-12) was synthesised using 3.9 g (0.0149 mol) of the Compound (XXII-12) according to Synthesis Example 31 (3). White solid, m.p.: 183-184 C., yield: 2.09 g, percent yield: 46.2%. IR KBr cm-1: 3382, 3268, 1482, 1344, 1230, 1164, 768. 1H-NMR (60 MHz, d6-DMSO, delta): 7.2-7.65 (5H, m, aromatic ring H*3, NH2), 7.86 (1H, dd, J=2Hx, 8 Hz, aromatic ring H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1535-75-7, its application will become more common.

Reference:
Patent; Kureha Kagaku Kogyo K.K.; US6610853; (2003); B1;,
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Related Products of 123652-95-9, 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. 123652-95-9, name is (3-Fluoro-4-methoxyphenyl)methanamine belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

6-Amino-N-(3-fluoro-4-methoxybenzyl)-2,5-dimethylthieno[3,2-e][1,2,4]triazolo[1,5-a]pyridine-7-carboxamide (Compound 2) In a vial equipped with a magnetic stir bar was added HATU (1.2 eq), compound E (1.0 eq), and DIEA (4.1 eq) in DMF (0.2 M). After 10 min, (3-fluoro-4-methoxyphenyl)methanamine (2.0 eq) was added. After 16 h, LCMS showed desired product. The reaction was passed through a syringe filter and purified by prep RP-HPLC Gilson, eluting 15-75% MeCN/water+0.1% TFA. Desired fractions were concentrated, in order to remove the acetonitrile. To the remaining aqueous mixture was added sat’d NaHCO3 and the mixture was extracted with EtOAc (3*). The collected organic layers were dried (MgSO4), filtered and concentrated to afford the desired product (37-48% yield). LCMS: RT=0.905 min, >98% 215 and 254 nM, m/z=400.2 [M+H]+. 1H NMR (400 MHz, d6-DMSO): delta 8.43 (t, J=5.8, 1H), 7.40 (s, 1H), 7.17-7.08 (m, 3H), 7.04 (s, 2H), 4.36 (d, J=5.8 Hz, 2H), 3.81 (s, 3H), 2.80 (s, 3H).

The synthetic route of (3-Fluoro-4-methoxyphenyl)methanamine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Vanderbilt University; Lindsley, Craig W.; Conn, P. Jeffrey; Engers, Darren W.; Jones, Carrie K.; Bridges, Thomas M.; Han, Changho; Felts, Andrew S.; (38 pag.)US2018/28501; (2018); A1;,
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Electric Literature of 946-80-5, 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. 946-80-5, name is Benzyl Phenyl Ether belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A. A 1.12 portion of anhydrous DMF is cooled to 0 C. and treated dropwise with 2.06 g of sulfuryl chloride. The resulting suspension is stirred for 30 min., then treated with 1.50 g of benzyl phenyl ether. The mixture is heated at 90 C. for 3 h, then cooled, extracted with brine and methylene chloride, and dried over MgSO4. Chormotography on silica gel (i-PrOH/hexanes) yields 4-benzyloxybenzenesulfonyl chloride.

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, Benzyl Phenyl Ether, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Vertex Pharmaceuticals Incorporated; US5723490; (1998); A;,
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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. 4463-59-6, name is 1-(2-Bromoethoxy)-2-methoxybenzene, A new synthetic method of this compound is introduced below., Quality Control of 1-(2-Bromoethoxy)-2-methoxybenzene

36 g(0.156 ml) of 2-(methoxyphenoxy)ethylbromide and 27.3 grams (0.186 mole) of phthalimide are dissolved in 100 ml of dimethylacetamide, and stirred with heat for diffusion to 90 C. After 30 minutes, 10.45 g(0.186 mole) of potassium hydroxide is dissolved in 30 ml of methanol solution for heating and diffusing over 1.5 hours. Upon cooling, the mixed solution is poured into 300 ml of water. After filtrating the extracted solids, 200 ml of 10% potassium carbonate solution is added, and stirred with heat. The paste-like substance obtained is filtrated. After rinsing with tap water several times, moisture-free alcohol is used for re-crystallization until while crystallization is obtained. 21 grams(0.071 mole) of the above product and 3.55 grams (0.071 mole) of hydrazine hydrate are dissolved in 70 ml of moisture-free alcohol, and upon heating and diffusing for 45 minutes, 20 ml of 18% hydrochloric acid is added into the mixture to continue the diffusion for one hour before cooling. After filtration, the residue obtained from reduction is mixed with 20% of sodium hydroxide for alkalization. Chloroform is used for extraction, and upon filtration and pressurized reduction, it is filled into the silicone tube for separation, while using ethyl acetate as the diluent to obtain an oily product, i.e. 2-(2-methoxy-phenoxy)ethylamine.

The synthetic route of 4463-59-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Chen, Ing-Jun; US2001/56211; (2001); A1;,
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Synthetic Route of 150-78-7,Some common heterocyclic compound, 150-78-7, name is 1,4-Dimethoxybenzene, molecular formula is C8H10O2, 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: Preparation of 2,5-dibromo-1 ,4-dimethoxybenzene (2); [00103] In a one liter round-bottom flask, a solution of bromine (35.2 g, 220 mmol) in chloroform (50 ml) was added dropwise to a solution of 1 ,4- dimethoxybenzene (13.8 g, 100 mmol) in chloroform (400 ml) under 00C. After stirring for 3 hours, 100 ml of saturated Na2CO3 solution was added. The organic layer was washed with water, brine, and dried over sodium sulfate. The solvent was removed on a rotary evaporator and the residue was performed recrystallization from ethanol to afford pure 2,5-dibromo-1 ,4- dimethoxybenzene (25.8 g, 85%). 1HNMR (CDCI3) 57.128 (s, 2 H), 3.873 (s, 6 H).

The synthetic route of 150-78-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AGENCY FOR SCIENCE, TECHNOLOGY AND RESEARCH; NATIONAL UNIVERSITY OF SINGAPORE; WO2006/93467; (2006); A1;,
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Reference of 17715-69-4, These common heterocyclic compound, 17715-69-4, name is 1-Bromo-2,4-dimethoxybenzene, 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 suspension of Pd2(dba)3 (6.9mg, 0.0075mmol), tBu3PHBF4 (8.7mg, 0.03mmol), KOH (42mg, 0.75mmol), aryl bromide 4 (0.36mmol) and tetralone 3 (0.3mmol) in a mixture of dioxane/water (4:1, v/v, 3mL) was degassed and heated under Ar and microwave irradiation (80W of initial power, 100°C, 40min, infrared probe). Then, the mixture was allowed to cool to rt, diluted in AcOEt, washed with saturated NH4Cl solution, dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure. The crude material was purified by silica gel chromatography. Dioxane quality is extremely important for the success of the reaction. Characterization of alpha-aryl-alpha-tetralones is given in Ref.[26].

Statistics shows that 1-Bromo-2,4-dimethoxybenzene is playing an increasingly important role. we look forward to future research findings about 17715-69-4.

Reference:
Article; Fernandes, Talita de A.; Costa, Paulo R. R.; Manvar, Dinesh; Basu, Amartya; Kaushik-Basu, Neerja; Domingos, Jorge L. O.; Nichols, Daniel Brian; European Journal of Medicinal Chemistry; vol. 112; (2016); p. 33 – 38;,
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Related Products of 41789-95-1, These common heterocyclic compound, 41789-95-1, name is 1-(3-Methoxyphenyl)-N-methylmethanamine, 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: Amine (1.2 equiv) and 3-bromotoluene (1 equiv) were added to an aqueous solution of TPGS-750-M-2% (1 mL/mmol). The mixture was degassed by bubbling Argon in through (5 min). NaO-t-Bu (1.5 equiv), of [(allyl)PdCl]2 (1.1%) and cBridp (4.4%) were added together to the previous solution. The mixture was stirred (at 1200 rpm) at 50 C (2-24 h). Volatiles were evaporated and the crude residue was purified by chromatographic column on silica gel using ethyl acetate and cyclohexane as solvent.

Statistics shows that 1-(3-Methoxyphenyl)-N-methylmethanamine is playing an increasingly important role. we look forward to future research findings about 41789-95-1.

Reference:
Article; Salome, Christophe; Wagner, Patrick; Bollenbach, Maud; Bihel, Frederic; Bourguignon, Jean-Jacques; Schmitt, Martine; Tetrahedron; vol. 70; 21; (2014); p. 3413 – 3421;,
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