Month: May 2021

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. 17715-69-4, name is 1-Bromo-2,4-dimethoxybenzene belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 1-Bromo-2,4-dimethoxybenzene

General procedure: A pyrex test tube containing solid of 1,3,5-trimethoxybenzene (1a, 0.3 mmol), carbon tetrabromide (0.075 mmol), AQN-2-CO2H (0.03 mmol) and dry EtOH (5 mL) was irradiated for 20 h at roomtemperature with stirring by a 21W fluorescent lamp under air. The reactionmixture was concentrated in vacuo, quenched with aq Na2S2O3 and extractedwith EtOAc. The organic layer was dried over MgSO4 and concentrated invacuo. Purification of the residue by flash chromatography on silica gel(hexane/ethyl acetate = 6:1) provided 2-bromo-1,3,5-trimethoxybenzene (2a)(66.8 mg, 90%,) as a white solid.

The synthetic route of 17715-69-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Tanaka, Masanori; Kamito, Yuji; Lei, Cui; Tada, Norihiro; Itoh, Akichika; Tetrahedron Letters; vol. 56; 43; (2015); p. 5886 – 5888;,
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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. 54314-84-0, name is ((3-Bromopropoxy)methyl)benzene, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 54314-84-0

To a solution of 3-(2,3,4,6-tetra-O-pivaloyl-beta-D-glucopyranosyloxy)-4-[2-(4-pivaloyloxyphenyl)ethyl]-1H-pyrazolo[3,4-b]pyridine (1 g) in acetone (10 mL) were added cesium carbonate (0.78g), benzyl 3-bromopropyl ether (0.32 mL) and a catalytic amount of sodium iodide, and the mixture was stirred at room temperature for 2 days. The reaction mixture was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate = 4/1 – 2/1) to give 1-(3-benzyloxypropyl)-3-(2,3,4,6-tetra-O-pivaloyl-beta-D-glucopyranosyloxy)-4-[2-(4-pivaloyloxyphenyl)ethyl]-1H-pyrazolo[3,4-b]pyridine (0.77g). This material was dissolved in methanol (10 mL). To the solution was added 10percent palladium-carbon powder (0.25 g), and the mixture was stirred at room temperature under a hydrogen atmosphere for 2 hours. The insoluble material was removed by filtration, and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate = 1/1 – 1/2) to give the title compound (0.54 g). 1H-NMR (CDCl3) delta ppm: 1.03 (9H, s), 1.14 (9H, s), 1.15 (9H, s), 1.17 (9H, s), 1.35 (9H, s), 1.9-2.1 (2H, m), 2.9-3.1 (2H, m), 3.1-3.35 (2H, m), 3.35-3.55 (2H, m), 3.95-4.1 (2H, m), 4.1-4.2 (1H, m) , 4.24 (1H, dd, J=12.4Hz, 1.7Hz), 4.49 (2H, t, J=6.1Hz), 5.2-5.3 (1H, m), 5.35-5.45 (1H, m), 5.45-5.55 (1H, m), 6.03 (1H, d, J=7.9Hz), 6.68 (1H, d, J=4.8Hz), 6.95-7.0 (2H, m), 7.15-7.2 (2H, m), 8.26 (1H, d, J=4.8Hz)

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 54314-84-0.

Reference:
Patent; Kissei Pharmaceutical Co., Ltd.; EP1724278; (2006); 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.

To a 250 mL flask, 2-bromoethyl ether (37.62 g, 0.246 mol),4-hydroxybenzaldehyde (32 g, 0.262 mol), anhydrous potassiumcarbonate (67.89 g, 0.491 mol) and 120 mL acetonitrilewere added. The solution was heated to reflux for 24 h.Then, the solvent was evaporated in vacuo and the residuewas dissolved in H2Oand extracted with ethyl acetate. Theorganic layers were washed with 2× 100 mL sodium hydroxidesolution (1 N) and with 2× 100 mL saturated brine,respectively. The obtained solution was concentrated to getthe pure product, yield 81%. 1H NMR (400 MHz, CDCl3)delta 9.72 (s, 1H, CHO), 7.68 (m, 2H, benzyl), 6.89 (m, 2H,benzyl), 4.05 (t, 2H, OCH2CH2O), 3.67 (t, 2H, OCH2CH2O),3.45 (q, 2H, -CH2CH3), 1.09 (t, 3H, CH3). Mass (ESI): calcdfor C11H14O3(M + H)+, 195.27; found 195.52.

Statistics shows that 1-Bromo-2-ethoxyethane is playing an increasingly important role. we look forward to future research findings about 592-55-2.

Reference:
Article; Wu, Fengshou; Yang, Mengqian; Zhang, Juan; Zhu, Sizhe; Shi, Mengge; Wang, Kai; Journal of Biological Inorganic Chemistry; vol. 24; 1; (2019); p. 53 – 60;,
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These common heterocyclic compound, 450-88-4, name is 1-Bromo-4-fluoro-2-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. SDS of cas: 450-88-4

Intermediate [Example Int15.101 -bromo-2-methoxy-4-(methylsulfanyl)benzeneTo a stirred solution of 1 -bromo-4-fluoro-2-methoxybenzene (4.0 mg) in DMF (40 mL) was added sodium methanethiolate (2.76 g). The mixture was stirred at room temperature for 30 minutes and at 85 C for 2 h. Water was added and the mixture was extracted with ethyl acetate. The organic phase was washed with saturated sodium chloride solution, dried (sodium sulfate) and the solvent was removed in vacuum. Silica gel chromatography gave 280 mg of the title compound.1 H-NMR (400MHz, DMSO-d6): delta [ppm]= 2.46 (s, 3H), 3.82 (s, 3H), 6.74 (dd, 1 H), 6.91 (d, 1 H), 7.44 (d, 1 H).

The synthetic route of 1-Bromo-4-fluoro-2-methoxybenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER SCHERING PHARMA AKTIENGESELLSCHAFT; KOPPITZ, Marcus; SCHULZE, Volker; KOSEMUND, Dirk; SCHIROK, Hartmut; BADER, Benjamin; LIENAU, Philipp; MARQUARDT, Tobias; WEGSCHEIDT-GERLACH, Christof; SIEMEISTER, Gerhard; PRECHTL, Stefan; WENGNER, Antje; BOeMER, Ulf; WO2011/64328; (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. 59557-91-4, name is 4-Bromo-2-methoxyaniline, A new synthetic method of this compound is introduced below., Recommanded Product: 59557-91-4

General procedure: 4-Bromobenzenamines 1a-c (6.4 mmol) were dissolved in the mixed solvents (2M K2CO3:DMF = 1:1, 24 mL), and then added corresponding 4-substituent phenylboronic acids 2a-h (7.7 mmol) and Pd (PPh3)4 (0.22 mmol) under argon. The reaction mixture was refluxed at 100 for 15 h (TLC monitored the reaction). The reaction was then cooled to room temperature and filtered. The filtrate was added 10 times the amount of water and extracted with ethyl acetate. The organic layer was washed with saturated NaCl solution, concentrated under reduced pressure, and dried to give a crude product. The crude product was purified by flash column chromatography (ethyl acetate/petroleum ether, 1:8-1:5) to afford 1,1′-biphenyl-4-amines 3a-x, yield: 77-95%.

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; Liu, Jingru; Ma, Ruxin; Bi, Fangchao; Zhang, Fa; Hu, Chaoyu; Venter, Henrietta; Semple, Susan J.; Ma, Shutao; Bioorganic and Medicinal Chemistry Letters; vol. 28; 10; (2018); p. 1825 – 1831;,
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Application of 41789-95-1, A common heterocyclic compound, 41789-95-1, name is 1-(3-Methoxyphenyl)-N-methylmethanamine, 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.

Step B: To a solution of the above amine (6.2 g, 41.00 mmol) from Step A in methylene chloride (100 mL) was added 3,4-dichlorophenacyl bromide (10.0 g, 37.3 mmol) and the resulting mixture was stirred at 0 0C for 1 hour prior to the addition of triethylamine (5.20 mL, 37.31 mmol), followed by 1 hour stirring at 0 0C. The reaction mixture was diluted with water (100 mL) then the aqueous phase was extracted with additional methylene chloride (3 x 75 mL). The combined extracts were dried over sodium sulfate, filtered, and concentrated to afford l-(3,4-dichlorophenyl)-2-((3- methoxybenzyl)(methyl)amino)ethanone (15.08 g) as a light yellow oil, which was used in the next step without further purification: 1H NMR (500 MHz, CDCl3) delta 8.08 (d, J = 2.0 Hz, IH), 7.78 (dd, J = 8.5; 2.0 Hz, IH), 7.50 (d, J = 8.5 Hz, IH), 7.25 (d, J= 8.5 Hz, IH), 6.90 (d, J= 7.5 Hz, IH), 6.87 (d, J= 2.5 Hz, IH), 6.82 (dd, J= 8.0; 2.5 Hz, IH), 3.79 (s, 3H), 3.66 (s, 2H), 3.60 (s, 2H), 2.33 (s, 3H).

The synthetic route of 41789-95-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ALBANY MOLECULAR RESERCH, INC.; WO2010/132442; (2010); 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. 171290-52-1, name is 3,5-Dimethoxyphenylacetylene, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 3,5-Dimethoxyphenylacetylene

General procedure: Azide 13 (300 mumol), alkyne (750 mumol), CuSO4 (9.6 mg, 60 mumol) and sodium ascorbate (60.0 mg, 300 mumol) were dissolved in 1:1 t-BuOH/H2O (3 mL). The mixture was stirred for 2 h at rt. After the completion of the reaction, the mixture was filtered and washed with H2O (70 mL) (solid A). The filtrate was extracted with EtOAc (3 * 70 mL). The combined organic extracts were dried over anhyd MgSO4, filtered, and concentrated by rotary evaporation (residue B). The solid A and residue B were combined and purified by column chromatography to afford 8 or 9.

According to the analysis of related databases, 171290-52-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Song, Doohee; Park, Yunjeong; Yoon, Jieun; Aman, Waqar; Hah, Jung-Mi; Ryu, Jae-Sang; Bioorganic and Medicinal Chemistry; vol. 22; 17; (2014); p. 4855 – 4866;,
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Synthetic Route of 701-07-5,Some common heterocyclic compound, 701-07-5, name is 2-(2′-Bromophenoxy)propane, molecular formula is C9H11BrO, 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.

[066] 3-methyl-N-(7H-pyrrolo[2,3-d]pyrimidin-2-yl)-2,3,4,S-tetrahydro-1H-benzo[d]- azepin-7- amineprepared in Step 7 was used without further purification.Asolution of 3-methyl-N-(7H- pyrrolo[2,3-d]pyrimidin-2-yl)-2,3,4,5-tetrahydro-1H-benzo[d]azepin-7-amine from Step 7(65 mg, crude, about 0.22 mmol), 1-bromo-2-isopropoxybenzene (57 mg, 0.27 mmol), (trans)cyclohexane-1,2-diamine (7.5 mg, 0.066 mmol), Cul (12 mg, 0.066 mmol), and K3P04 (164 mg, 0.77 mmol) in dioxane (2 mL) was stirred at 120 C under nitrogen overnight. The mixture was diluted with water (5 mL), and extracted with EtOAc (20 mL). The organic layer was washed with brine (10 mL), dried over Na2504, filtered, and concentrated. The residue was purified byprep-TLC to give the title compound N-(7-(2-isopropoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-2- yl)-3-methyl-2,3,4,S-tetrahydro-1H-benzo[d]azepin-7-amine(9 mg, yield: 9%).

The synthetic route of 701-07-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CHANGZHOU JIEKAI PHARMATECH CO., LTD.; ZHANG, Jintao; XIANG, Yibin; XU, Wen; JIAN, Shanzhong; (40 pag.)WO2015/143692; (2015); A1;,
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Synthetic Route of 6851-80-5, These common heterocyclic compound, 6851-80-5, name is 1-(2-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: To a suspension of the corresponding secondary amine (3.22 mmol) and anhydrous K2CO3 (765 mg, 5.48 mmol) in CH3CN (20 mL) was added the intermediates 3-5 (0.60 mmol). The mixture was refluxed for 6-8 h. The solvent was removed under reduced pressure. The residue was diluted with water (30 mL) and the mixture was extracted with dichloromethane (30 mL×3). The combined organic phases were washed with brine, dried over sodium sulfate, filtered and concentrated under reduced pressure. The residue was purified on a silica gel chromatography in petroleum ether/acetone (20/1, v/v) to afford compound 7-9

Statistics shows that 1-(2-Methoxyphenyl)-N-methylmethanamine is playing an increasingly important role. we look forward to future research findings about 6851-80-5.

Reference:
Article; Song, Qing; Li, Yan; Cao, Zhongcheng; Qiang, Xiaoming; Tan, Zhenghuai; Deng, Yong; Bioorganic Chemistry; vol. 84; (2019); p. 137 – 149;,
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Related Products of 89282-70-2, 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. 89282-70-2, name is 2-Methoxy-2-methylpropan-1-amine belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Preparation 3 Synthesis of N-(2-methoxy-2-methylpropyl) formamide Formic acid (19.2 g, 0.40 mol) and acetic anhydride (40.8 g, 0.40 mol) Were combined and heated to 45-50 C. for one hour and cooled to approximately 0 C. in an ice/acetone bath. A solution of 2-methoxy-2-methylpropyl-1-amine (36 g, 0.35 mol), precooled to approximately 0 C. in an ice/acetone bath was added slowly while keeping the temperature of the mixture below 12 C. After the addition was complete, the mixture was allowed to warm slowly to room temperature and was stirred at room temperature overnight. The solution was evaporated and the residue distilled at 97-107 C./1-2 mm Hg. to give 43.2 g (94%). NMR (CDCl3): delta 1.2 (s, 6H, CH3), 3.3 (m, 5H, CH3 O and CH2), 6.6 (b, 1H, NH), 8.2 (bs, 1H, HCO).

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-Methoxy-2-methylpropan-1-amine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; E. I. Du Pont de Nemours and Company; US4988827; (1991); A;,
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