Month: June 2021

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. 126-38-5, name is 1-Bromo-2,2-dimethoxypropane, A new synthetic method of this compound is introduced below., Application In Synthesis of 1-Bromo-2,2-dimethoxypropane

To a suspension of 5-bromo-3-methylpyrazin-2-amine (4.63g, 24.6 mmol) in iPrOH (30 ml) was added l-bromo-2,2-dimethoxypropane (3.66 ml, 27.1 mmol), pyridinium para-toluene sulfonic acid (0.62g, 2.5 mmol) and the mixture heated to 65C in a sealed tube for 36h. The reaction was diluted with DCM, washed with saturated sodium hydrogen carbonate solution, dried (Na2S04) and concentrated. Purification by flash column chromatography on silica gel (EtOAc: Hept 1:4-1: 1) afforded the titled product as a light yellow crystalline solid (3.96 g, 71%). MS (m/e): 226.1 (M+H+, Br)

The synthetic route of 126-38-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; GREEN, Luke; PINARD, Emmanuel; RATNI, Hasane; WILLIAMSON, Patrick; (95 pag.)WO2015/197503; (2015); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

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. 216067-66-2, name is O-(2,4-Dimethoxybenzyl)hydroxylamine, A new synthetic method of this compound is introduced below., Formula: C9H13NO3

INTERMEDIATE 2 Preparation of 5- (4-Formvl-phenvl)-furan-2-carboxylic acid (2, 4-dimethoxv-benzyloxv)- amide 0- (7-Azabenzotriazol-1-yl)-N, N, N’, N’-tetramethyluronium hexafluorophosphate (HATU, 6.6 g) and 5- (4-Formyl-phenyl)-furan-2-carboxylic acid (3.14 g, was made by method analogous to INTERMEDIATE 1, but suing appropriate starting material and the methyl ester was hydrolyse to the acid) were added to the solution of 0- (2, 4-Dimethoxy-benzyl)- hydroxylamine (2.64 g) and DIEA (6.26 mL) in DMF (60 mL) at 0C, and stirred at the same temperature for about 1h. After the TLC showing the substances disappeared, saturated sodium bicarbonate was added to the reaction mixture, and stirred for additional 1h, worked up to give a yellow oil. The oil was dissolved in small amount of THF, then diluted with water (the oil appeared again), under vigorous stirring ether was added, the oil solidified soon. The solid was filtered and washed with water and ether. The solid was recrystallized from methanol/ether to give 3.8 g of 5- (4-Formyl-phenyl)-furan-2-carboxylic acid (2, 4-dimethoxy-benzyloxy)-amide.

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; S*BIO PTE LTD; WO2005/40161; (2005); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Electric Literature of 22094-18-4, A common heterocyclic compound, 22094-18-4, name is 1,3-Dibromo-2,2-dimethoxypropane, molecular formula is C5H10Br2O2, 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 129A 3,3-dimethoxy-1-[4-(trifluoromethoxy)phenyl]cyclobutanecarboxamide 2-[4-(Trifluoromethoxy)phenyl]acetonitrile (7.86 mL, 50 mmol), 1,3-dibromo-2,2-dimethoxypropane (13.10 g, 50.0 mmol), and sodium tert-butoxide (10.57 g, 110 mmol) were dissolved in DMSO (100 mL) and water (5 mL), and the mixture was heated for 1 hour at 125 C. The reaction was cooled to ambient temperature and stirred overnight. The reaction mixture was diluted with water and extracted three times with diethyl ether. The combined organic layers were washed with brine, dried with MgSO4, filtered, and concentrated to give the title compound (17.02 g, 53.3 mmol, 107% yield). MS (DCI+): m/z 320.1 (M+H), 337.1 (M+NH4). 1FINMR (300 MHz, DMSO-d6) delta 7.44 (d, J=8.8 Hz, 2H), 7.34 (s, 1H), 7.31 (d, J=8.8 Hz, 2H), 6.90 (s, 1H), 3.05 (s, 3H), 3.02-2.93 (m, 5H), 2.41 (d, J=13.4 Hz, 2H).

The synthetic route of 22094-18-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AbbVie Inc.; Bayburt, Erol K.; Clapham, Bruce; Cox, Phil B.; Daanen, Jerome F.; Dart, Michael J.; Gfesser, Gregory A.; Gomtsyan, Arthur; Kort, Michael E.; Kym, Philip R.; Schmidt, Robert G.; Voight, Eric A.; US2014/80803; (2014); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

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. 349-65-5, name is 2-Methoxy-5-(trifluoromethyl)aniline, A new synthetic method of this compound is introduced below., Product Details of 349-65-5

The 1-(5-bromopyridin-2-yl)-3-(2-methoxy-5-trifluoromethylphenyl)urea can be prepared in the following way: A solution of 11.05 g (57.80 mmol) of 2-methoxy-5-trifluoromethylaniline in 100 ml of anhydrous tetrahydrofuran is added, at 0 C. over 3 minutes, to a solution of 6 g (20.23 mmol) of triphosgene in 500 ml of anhydrous tetrahydrofuran. 16.50 ml (116.80 mmol) of triethylamine are added at 0 C. The reaction is stirred at 0 C. for 10 minutes and then at ambient temperature for 1 h 45 min. A solution of 10 g (57.80 mmol) of 2-amino-5-bromopyridine in 100 ml of anhydrous tetrahydrofuran is then added at ambient temperature. The reaction is stirred at ambient temperature for 20 h. The mixture is filtered over sintered glass and the white solid obtained is washed with tetrahydrofuran and a small amount of ethyl acetate. The filtrate is evaporated to dryness under reduced pressure and a pale yellow solid is obtained. The latter is triturated with ethyl acetate and water and then, after filtration over sintered glass, 12.04 g of 1-(5-bromopyridin-2-yl)-3-(2-methoxy-5-trifluoromethylphenyl)urea are obtained in the form of a white solid. EI: m/z=389 (M+), m/z=191 (C8H8NOF3+), m/z=172 (C5H5N2Br+) base peak.

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; AVENTIS PHARMA S.A.; US2007/259910; (2007); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

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;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

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;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

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;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

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;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

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;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

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;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem