Author: Jessica.F

Application of 1535-75-7, 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 1535-75-7 as follows.

A solution of 2.09 g of 2-trifluoromethoxyaniline and 3.15 g of 1-(2-chloroethyl)-4-(2-methoxyphenyl)-piperazine in 20 ml of n-butanol was stirred at 100C for 2 hours. The mixture was then cooled, diluted with water, alkalinised with 2N sodium hydroxide and extracted with chloroform. The organic phase was dried on anhydrous sodium sulphate, evaporated until dry and the crude purified via flash chromatography (ethyl acetate : petroleum ether 3:7) and subsequently crystallised from ethanol giving 0.55 g (12%) of 1-[N-(2-trifluoromethoxyphenyl)-2-aminoethyl]-4-(2-methoxyphenyl)-piperazine. Melting point: 69.5-71C.1H-NMR (CDCl3, delta): 8.02-7.85 (br, 1H, NH), 7.43-7.27 (m, 2H, aniline CHs), 7.03-6.80 (m, 4H, methoxyphenyl ring CHs), 6.72 (dd, 1H, aniline CH), 6.57 (t, 1H, aniline CH), 3.86 (s, 3H, OCH3), 3.43-3.23 (m, 2H, NHCH2CH2), 3.23-3.03 (m, 4H, piperazine protons), 2.85-2.60 (m, 6H, piperazine protons and NHCH2CH2). The title compound was prepared following the procedure described in Example I, second step, except that 1-[N-(2-trifluoromethoxyphenyl)-2-aminoethyl]-4-(2-methoxyphenyl)-piperazine, prepared as described above, was used in place of 1-[N-(2-nitrophenyl)-2-aminoethyl]4-(2-methoxyphenyl)-piperazine and that 4-dimethylaminopyridine was used in place of triethylamine, the mixture being heated for 1.5 h at reflux. The crude material was purified via flash chromatography (ethyl acetate : petroleum ether 4:6). Yield: 44%.1H-NMR (CDCl3, delta): 7.48-7.25 (m, 4H, trifluoromethoxyaniline ring CHs), 7.02-6.81 (m, 4H, methoxyphenyl ring CHs), 4.40-4.20 (m, 1H, C(O)NCH(H)CH2), 3.84 (s, 3H, OCH3), 3.36-3.18 (m, 1H, C(O)NCH(H)CH2), 3.10-2.90 (m, 4H, piperazine protons), 2.75-2.45 (m, 6H, piperazine protons and C(O)NCH2CH2), and 2.03-1.80 (m, 1H, CHC(O)), 1.75-0.80 (m, 10H, cyclohexyl protons).

According to the analysis of related databases, 1535-75-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; RECORDATI S.A.; RECORDATI INDUSTRIA CHIMICA E FARMACEUTICA S.p.a.; EP1000047; (2003); B1;,
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Related Products of 143-24-8, 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. 143-24-8, name is 2,5,8,11,14-Pentaoxapentadecane, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: Crystals of[Li(glyme)][B(GlyPr2)2] (except 4a) were obtained by recrystallizationat 25 C using solvate 3 and the correspondingglyme (520equiv. per Li). Crystals of solvate 4a were grownfrom a DME solution of 3 and pentane at 25 C

The chemical industry reduces the impact on the environment during synthesis 2,5,8,11,14-Pentaoxapentadecane. I believe this compound will play a more active role in future production and life.

Reference:
Article; Oishi, Masataka; Kajiwara, Meisetsu; Bulletin of the Chemical Society of Japan; vol. 91; 1; (2018); p. 12 – 18;,
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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.

[00330] To a solution of compound 2, 19 and Et3N in DMF at rt. then HATU was added at rt.After stirring for lh at rt, the reaction was diluted with water and extracted with EA, washed byK2C03 and brine, dried over Na2SO4 and concentrated and purified by FCC to afford compound20. ?H NMR (400 MHz, CDC13): 3 8.46 (s, 1H), 8.42 (s, 1H), 7.10-7.06 (m, 2H), 6.94-6.90 (m,1H), 6.47-6.44 (m, 1H), 4.57 (d, J = 6.0 Hz, 2H), 3.87 (s, 3H); mlz (ESI+) (M+H)+ = 313.05.

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, (3-Fluoro-4-methoxyphenyl)methanamine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; THE BOARD OF TRUSTEES OF THE LELAND STANFORD JUNIOR UNIVERSITY; YANG, Wenjin; CHEN, Che-Hong; MOCHLY-ROSEN, Daria; WO2014/160185; (2014); A2;,
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Related Products of 29578-39-0, These common heterocyclic compound, 29578-39-0, name is 1-Bromo-3-fluoro-5-methoxybenzene, 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.

To a solution of 9-1 (20 g, 97.55 mmol) in tetrahydrofuran (100 mL) was added dropwise n-butyl lithium (43 mL, 2.5 M, 107.3 mmol) at -78 C. It was stirred for 30 minutes and N,N- dimethylformamide (15.1 mL, 195.1 mmol) was added at this temperature. It was stirred for another 30 minutes and the cold bath was removed. After 1 hour, the reaction was quenched with saturated aqueous ammonium chloride. The organic layer was washed with water and saturated aqueous sodium chloride, dried (sodium sulfate), filtered and concentrated. The residue was purified by chromatography on silica to give 9-2.

Statistics shows that 1-Bromo-3-fluoro-5-methoxybenzene is playing an increasingly important role. we look forward to future research findings about 29578-39-0.

Reference:
Patent; BIOTICA TECHNOLOGY LIMITED; GREGORY, Matthew Alan; MOSS, Steven James; WO2013/61052; (2013); A1;,
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Related Products of 22236-10-8, The chemical industry reduces the impact on the environment during synthesis 22236-10-8, name is 4-(Difluoromethoxy)aniline, I believe this compound will play a more active role in future production and life.

Step A: 6-(difluoromethoxy)benzo[d]thiazol-2-amine To 4-(difluoromethoxy)aniline (9.55 g, 60 mmol) in acetic acid (90 niL) was added potassium thiocyanate (KSCN) (12.41 mL, 240 mmol). The mixture was stirred for 20 minutes (KSCN dissolved into solution). To this mixture bromine (3.08 mL, 60.0 mmol) in acetic acid (40 mL) was added dropwise over 20 minutes. The reaction was stirred at room temperature overnight. It was poured into a mixture of 800 ml ice water and 200 ml saturated ammonium hydroxide. The product was extracted with ethyl acetate (5x). The organics were combined, washed with brine, dried over sodium sulfate, filtered and concentrated in vacuo to afford 6-(difluoromethoxy)benzo[d]thiazol-2-amine (12.6 g, 52.4 mmol, 87 % yield) as a yellow solid.

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, 4-(Difluoromethoxy)aniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; COOK II, James H.; MCDONALD, Ivar, M.; KING, Dalton; OLSON, Richard, E.; WANG, Nenghui; IWUAGWU, Christiana, I.; ZUSI, Christopher, F.; MACOR, John, E.; WO2011/53292; (2011); 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. 349-55-3, name is 3-Methoxy-5-(trifluoromethyl)aniline, A new synthetic method of this compound is introduced below., Product Details of 349-55-3

EXAMPLE 33 Preparation of 4-[(3-methoxy-5-trifluoromethyl phenyl)hydrazono]-4H-pyrazole-3,5-diamine In a manner similar to that described in Example 2,4-[(3-methoxy-5-trifluoromethylphenyl)hydrazono]-4H-pyrazole-3,5-diamine was prepared using 134 mg (0.5 mmol) of 2-[(3-methoxy-5-trifluoromethylphenyl)hydrazono]malononitrile, which was derived from 3-methoxy-5-trifluoromethylaniline (191 mg, 1.0 mmol) and malononitrile (1.5 mmol), and hydrazine hydrate. Very little solid had formed after heating the reaction at 75 C. for 1 hr, however, analysis of the reaction solution by TLC indicated that no starting material remained. The solution was allowed to cool to ambient temperature and the solvent was evaporated. The residue was dissolved in ethyl acetate and then precipitated by the addition of hexanes. The resulting solid was isolated by filtration and dried to yield 10 mg (7%) of the title compound as a yellow solid.

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; Zhang, Zaihui; Daynard, Timothy Scott; Sviridov, Serguei V.; Chafeev, Mikhail A.; Wang, Shisen; US2003/60453; (2003); A1;,
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Electric Literature of 6298-96-0, A common heterocyclic compound, 6298-96-0, name is 1-(4-Methoxyphenyl)ethylamine, molecular formula is C9H13NO, 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 mixture of (S)-1-(4-methoxyphenyl)-ethylamine (475 mg) and 6-chloropurine riboside (300 mg) in PrOH (70 ml) was heated to 70 C. and reacted for 8 h. After evaporation of the reaction mixture, the residue was separated by column chromatography over Sephadex LH-20 gel and eluted with ethanol to yield N6-[(S)-1-(4-methoxyphenyl)-ethyl]adenosine (345 mg) as a white solid: positive ESIMS m/z 402 [M+H]+ and 424 [M+Na]+; 1H NMR (300 MHz, DMSO-d6): the adenosine moiety delta 8.38 (1H, s, H-2), 8.23 (1H, brs, -NH), 8.18 (1H, s, H-8), 5.90 (1H, d, J=6.3 Hz, H-1′), 5.46 (1H, d, J=6.3 Hz, -OH), 5.42 (1H, m, -OH), 5.20 (1H, d, J=4.5 Hz, -OH), 4.61 (1H, m, H-2′), 4.16 (1H, m, H-3′), 3.98 (1H, m, H-4′), 3.66 (1H, m, H-5’a), 3.54 (1H, m, H-5’b); the (S)-1-(4-methoxyphenyl)-ethyl moiety delta 7.35 (1H, d, J=8.4 Hz, H-2″, H-6″), 6.84 (1H, d, J=8.4 Hz, H-3″, H-5″), 5.48 (1H, m, H-7″), 3.71 (3H, s, -OCH3), 1.51 (3H, d, 7.2 Hz, H-8″); 13C NMR (75 MHz, DMSO-d6): the adenosine moiety 5153.9 (s, C-6), 152.3 (d, C-2), 148.6 (s, C-4), 139.8 (d, C-8), 119.7 (s, C-5), 88.0 (d, C-1′), 85.9 (d, C-4′), 73.6 (d, C-2′), 70.7 (d, C-3′), 61.7 (t, C-5′); the (S)-1-(4-methoxyphenyl)-ethyl moiety delta 158.0 (s, C-4″), 137.1 (s, C-1″), 127.3 (d, C-2″, C-6″), 113.6 (d, C-3″, C-5″), 55.0 (q, -OCH3), 48.2 (d, C-7″), 22.5 (q, C-8″).

The synthetic route of 6298-96-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; INSTITUTE OF MATERIA MEDICA, CHINESE ACADEMY OF MEDICAL SCIENCES; Shi, Jiangong; Zhang, Jianjun; Yue, Zhenggang; Li, Min; Zhu, Chenggen; Zhang, Ying; Zi, Jiachen; Wang, Yafang; Fan, Xiaona; Xu, Ruiming; Lin, Sheng; Li, Yan; Yang, Yongchun; Sheng, Li; US2013/45942; (2013); A1;,
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Adding a certain compound to certain chemical reactions, such as: 111-95-5, name is Bis(2-methoxyethyl)amine, 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 111-95-5, HPLC of Formula: C6H15NO2

Propargyl bromide (17.8g, 150mmol) was added dropwise to a mixture of bis(2-methoxy-ethyl)amine (20g, 150mmol) and cesium carbonate (49g, 150mmol) in 350mL of acetone. The mixture was stirred overnight under nitrogen at room temperature. The inorganic salts were then filtered off, and the solvent was removed. The residue was dissolved in saturated sodium bicarbonate solution and extracted with ethyl acetate. The organic extracts were then evaporated to give 20g of bis-(2-methoxy-ethyl)-prop-2-ynyl-amine: mass spectrum (m/e): M+H 172.

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, Bis(2-methoxyethyl)amine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Wyeth Holdings Corporation; EP1950201; (2008); A1;,
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Reference of 101-84-8,Some common heterocyclic compound, 101-84-8, name is Diphenyl oxide, molecular formula is C12H10O, 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.

The reactor was charged with 3.16 g of AlCl3 and 711 g of bromine. Diphenyl oxide (46.1 g, 0.271 mol) and the Br2/Cl2 mixture (BrCl) were cofed to the reactor during 124 minutes at 55 C to 57 C. The rate of addition was at a proportion of about 8.2 g Br2/Cl2 mixture (BrCl) per gram of DPO, such that the addition of both was completed at the same time. The mixture in the reactor was refluxed for 10 minutes after the cofeeds had ended, and deionized H2O was added. The reactor was set for distillation. The halogen (mostly Br2, but also comprised of BrCl and Cl2) was distilled off. When most of the halogen was gone, more deionized water was added. The remaining halogen was distilled off to 1000C. The remaining mixture was cooled to 6O0C, and 30 mL of 25% NaOH was added to pH 13-14. The resultant mixture was filtered and washed well with deionized water. A sample was subjected to GC analysis. The GC trace showed the product to contain 0.26% Br9DPO (meta and para hydrogen isomers only), 2.52% Br9ClDPO, and 97.2% Br10DPO. None (less than 0.02%) of the ortho hydrogen isomer of Br9DPO was detected. The sample was oven dried. [0043] The drawings show illustrative GC traces formed using the recommended gas chromatographic procedure described hereinabove. In these traces, the abscissa is time in minutes and the ordinate is the detector response. A copy of the GC trace of the product formed in Example 1 appears as Fig. 1. In Fig. 1, the peak at 1.358 represents the area percentage of what is deemed to be the meta and para isomers of nonabromodiphenyl oxide. No peak for the ortho-isomer of nonabromodiphenyl oxide was observed. The peaks at 2.103 and 2.200 were deemed to be Br9ClDPO isomers. The peak at 2.649 represents the area percentage of decabromodiphenyl oxide.

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

Reference:
Patent; ALBEMARLE CORPORATION; WO2008/27780; (2008); 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. 592-55-2, name is 1-Bromo-2-ethoxyethane, A new synthetic method of this compound is introduced below., category: ethers-buliding-blocks

Weigh 2,6-diaminopurine nucleoside (CAS No.: 2096-10-8) and dissolve 135.58kg in 1350L DMF.The reaction solution is cooled to 0 ± 2 C,Add NaH 29.10kg under argon protection.The temperature of the addition process was 0 C to 5 C, and the mixture was stirred at 0 C for 1 h.After the above reaction system naturally returns to room temperature,Drop into the system2-bromoethyl ethyl ether 73.64 kg,The reaction was stirred at room temperature.The reaction to the product no longer increases.The water quenching reaction was slowly added to the system at 0 ± 2 C.A 2 M HCl solution was slowly added to the system to adjust the pH to neutral.Concentrate in a vacuum at 65 C until it drops.The residual solid is crystallized in ethanol72.91kg of pale yellow solid,It is a 2′-EOE-2,6-diaminopurine nucleoside.The purity was 98.3%, and the yield was 42.8%.

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

Reference:
Patent; Shanghai Zhaowei Science And Technology Co., Ltd.; Shanghai Zhaowei Biological Engineering Co., Ltd.; Sun Bo; Li Xiqun; Zheng Weijian; Chen Hongyu; (10 pag.)CN108822174; (2018); A;,
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