Month: June 2021

Synthetic Route of 7589-27-7, 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. 7589-27-7, name is 2-(4-Fluorophenyl)ethanol. A new synthetic method of this compound is introduced below.

Example 316 Synthesis of 2-(4-fluorophenyl)acetaldehyde To a stirred suspension of pyridinium chlorochromate (6.9 g, 21.4 mmol) in CH2Cl2 (100 ml) was added a solution of 2-(4-fluorophenyl)ethanol (3.0 g, 21.4 mmol) in CH2Cl2 (10 ml). The resulting suspension was stirred for 2 hours at room temperature and was then diluted with ether. The resulting suspension was filtered through a pad of Celite and washed with ether. The solvents were removed under reduced pressure to yield the crude title compound as a green oil (2.6 g, 86%), which was used as such for further reaction. 1H NMR (300 MHz, CDCl3, 25 C.): b=9.75 (s, 1H, CH), 7.19-7.22 (m, 2H, PhH), 7.06 (t, J=8.5 Hz, PhH), 3.68 (s, 2H, CH2) ppm.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,7589-27-7, 2-(4-Fluorophenyl)ethanol, and friends who are interested can also refer to it.

Reference:
Patent; KATHOLIEKE UNIVERSITEIT LEUVEN, K.U.LEUVEN R&D; De Jonghe, Steven; Gao, Ling-Jie; Herdewijn, Piet; Herman, Jean; Jang, Miyeon; Leyssen, Pieter; Louat, Thierry; Neyts, Johan; Pannecouque, Christophe; Vanderhoydonck, Bart; US2013/190297; (2013); A1;,
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Related Products of 148043-73-6, 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. 148043-73-6, name is 4,4,5,5,5-Pentafluoropentan-1-ol. A new synthetic method of this compound is introduced below.

Synthesis of compound 17 A 250 ml flask containing a solution of compound 18 (20 g, 1 12.3 mmol) in 50 ml of dry acetonitrile under inert nitrogen atmosphere. Triethylamine (19.9 ml, 142.6 mmol) and a solution of Methanesulfonyl chloride (9.9 ml, 128 mmol) in 35 ml ACN were slowly added at a temperature below 20 C. The mixture was stirred at room temperature 4 h. The mixture was concentrated by evaporating most of the ACN and extracted with CH2CI2. The organic phase was washed with saturated NaCI solution, dried over anhydrous MgS04, filtered and evaporated to dryness. 24.45 g of a yellow liquid was obtained (122% by mass).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,148043-73-6, 4,4,5,5,5-Pentafluoropentan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; CRYSTAL PHARMA, S.A.U.; PEREZ ENCABO, Alfonso; TURIEL HERNANDEZ, Jose Angel; GALLO NIETO, Francisco Javier; LORENTE BONDE-LARSEN, Antonio; GARCIA ESCUDERO, Luis Angel; WO2015/181116; (2015); A1;,
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Synthetic Route of 722-92-9, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 722-92-9, name is 2-(4-Aminophenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol, molecular formula is C9H7F6NO, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

To the stirred solution of 2-(4-aminophenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol (1.0 g, 3.86 mmol) in dry tetrahydrofuran (THF) under inert atmosphere, triphenylphosphine (3.04 g, 11.58 mmol) was added and stirred for 20 minutes. (E)-Diisopropyl diazene-1,2- dicarboxylate (0.936 g, 4.63 mmol) and methanol (0.23 mL, 5.79 mmol) were added to the reaction mixture at 0-5 °C. The reaction mixture was refluxed for 4-5 hours. Aftercompletion of the reaction, the reaction mixture was diluted with methylene chloride and purified using column chromatography (silica gel, hexane and ethyl acetate).

According to the analysis of related databases, 722-92-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; PIRAMAL ENTERPRISES LIMITED; SHARMA, Rajiv; SAHU, Bichismita; MALI, Sunil, Vasantrao; SINGH, Deepak; KUMAR, Pramod, Bhaskar; DAWANGE, Mahesh; MISTRY, Hitesh; (108 pag.)WO2015/145371; (2015); A1;,
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Adding a certain compound to certain chemical reactions, such as: 78573-45-2, 3-(3-(Trifluoromethyl)phenyl)propan-1-ol, 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, Computed Properties of C10H11F3O, blongs to alcohols-buliding-blocks compound. Computed Properties of C10H11F3O

Example 20; [00088] 3.0 g of crude material of compound V were dissolved in DCM (60 ml). TEA (5.6 ml) was added followed by drop-wise addition of Methanesulfonyl chloride (1.2 ml) at room temperature. The reaction mixture was stirred at room temperature for 2 hours. Then the reaction mixture was poured into crushed ice (98 g) and INHCl (30 ml). DCM (30 ml) was added to the mixture. Phase separation was done and the aqueous phase was extracted with DCM (30 ml) once again. The organic phase was EPO dried over Sodium sulfate and the solvent was evaporated under vacuum to give 3.39 g of the compound VI.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,78573-45-2, 3-(3-(Trifluoromethyl)phenyl)propan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; TEVA PHARMACEUTICAL INDUSTRIES, LTD.; TEVA PHARMACEUTICALS USA, INC.; WO2006/125026; (2006); A2;,
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Electric Literature of 3068-00-6, Adding some certain compound to certain chemical reactions, such as: 3068-00-6, name is 1,2,4-Butanetriol,molecular formula is C4H10O3, 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 3068-00-6.

To a 500 ml_ flask, 1 ,2,4-trihydroxybutane (III, 159 g, 1.5 mol, 1 equ.) and p-toluenesulfonic acid monohydrate (1.5 g, 8.72 mmol, 0.006 equ.) were added. The solution was heated to 160-180 C. Reaction was monitored by GC. The resulting mixture was purified by fractional distillation to give 3-OH-tetrahydrofuran as colorless oil (120.5 g 91.3% yield): bp 86-88 C (23 mmHg) 1H NMR (400 MHz, CDCI3) delta 4.43-4.42 (1 H, t), 3.95-3.67 (4H, m), 3.08- 3.07 (1 H, d), 2.07-1.82 (2H, m). GCMS m/z 88 (M+).

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. 3068-00-6, 1,2,4-Butanetriol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL TRADING (SHANGHAI) CO., LTD; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; XING, Lidong; DONG, Weitong; LU, Jun; SCHOLZ, Ulrich; YAN, Jun; YANG, Jinsong; WO2014/140017; (2014); A1;,
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Electric Literature of 1562-00-1, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 1562-00-1, name is Sodium isethionate, molecular formula is C2H5NaO4S, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Preparation of Dowex 1×8 HES. Dowex 1×8 Cl (5 g) was suspended in a minimum amount of water (10 mL), stirred for 10 min and filtered. The residue was suspended in a freshly prepared sodium isethionate (3.7 g, 25 mmol) solution in water (10 mL). The mixture was stirred for 10 min, filtered and the residue was washed with water (50 mL x 3) and methanol (50 mL x 3) successively. The resin was dried by vacuum suction for 15 min to give Dowex 1×8 isethionate (4.0 g, 0.96 milliequivalent/g).Synthesis of COHPyrv-24-HES. To a solution of CoHPyrv-24 (30 mg, 0.04 mmol) in 50:50, MeOH: H20 (1 .5 ml.) was added Dowex 1×8 isoethionate (0.21 g, 0.2 meq) and the mixture was stirred at room temperature for 30 min. The resulting mixture was then filtered and washed with water, 50:50 Me()H 20 and MeOH successively (50 mL total vol .) until the resin turned colorless. The filtrate was concentrated and dried under high vacuum to give 29 mg of the title compound.

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 1562-00-1, Sodium isethionate.

Reference:
Patent; CITY OF HOPE; JONES, Jeremy; PAL, Sumanta, Kumar; (187 pag.)WO2017/41040; (2017); A1;,
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The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 756520-66-8, name is 1-(2,6-Dichloro-3-fluorophenyl)ethanol. This compound has unique chemical properties. The synthetic route is as follows. Safety of 1-(2,6-Dichloro-3-fluorophenyl)ethanol

182 g of Compound 2 and 135 g of phthalic anhydride were dissolved in 124 mL of triethylamine, and 2 g of 4-dimethylaminopyridine (DMAP) was added.After refluxing for 2 hours, the heating was stopped.Cool to about 50 C and add 40 mL of ethyl acetate.Then adjust the pH to about 1.5 with 2N hydrochloric acid.Stir for another half an hour,a lot of white solids appear,Filter and wash twice with water,Compound 3 was obtained in a yield of 93%.The content is 98.5%.

With the rapid development of chemical substances, we look forward to future research findings about 756520-66-8.

Reference:
Patent; Kairuiside Biochemical (Suzhou) Co., Ltd.; Wu Shengwen; Wu Lei; Song Qianqian; (6 pag.)CN109438180; (2019); A;,
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Related Products of 2807-30-9, 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. 2807-30-9, name is 2-Propoxyethanol. A new synthetic method of this compound is introduced below.

General procedure: p-Toluensulfonyl chloride (2.6 g, 0.014 mol) was slowly added to the mixture of appropriate2-alkoxyethanol respectively (oxiran-2-yl)methanol (0.014 mol) and triethylamine (1.84 g, 0.018 mol) indichlormethane (20 mL) cooled at 0 C. The mixture was then stirred for 1 h at ambient temperature.The precipitate was filtered and the organic phase was washed with 2 M HCl, saturated solutionof Na2CO3 and water, dried over MgSO4, and then the solvent was evaporated. Product T2 wasrecrystallized from petroleum ether/diethyl ether in ratio 5:1.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,2807-30-9, its application will become more common.

Reference:
Article; Marvanova, Pavlina; Padrtova, Tereza; Odehnalova, Klara; Hosik, Ondrej; Oravec, Michal; Mokry, Petr; Molecules; vol. 21; 12; (2016);,
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Electric Literature of 3637-61-4, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.3637-61-4, name is Cyclopentanemethanol, molecular formula is C6H12O, molecular weight is 100.16, as common compound, the synthetic route is as follows.

General procedure: Ionic liquid [Dsim]HSO4 (6.5 mg, ?0.02 mmol) was added to a stirred mixture of alcohol, phenol or naphthol (1.0 mmol) and HMDS (80 mg, 0.5 mmol) at room temperature under solvent free conditions. After completion of the reaction (monitored by TLC, It should be noted that when addition of HMDS is finished stirring of the mixture is stopped after 1 min. TLC showed that in most of the cases the reaction is completed immediately after the addition of HMDS), the product was extracted with Et2O and the ionic liquid was recovered and was dried at 65 ?C under vacuum to remove moisture, and then reused. Evaporation of the solvent under reduced pressure gave the highly pure product without further purification. The desired pure products were characterized by comparison of their IR, NMR and MS data as well as boiling poin twith those of known compounds

The chemical industry reduces the impact on the environment during synthesis 3637-61-4, I believe this compound will play a more active role in future production and life.

Reference:
Article; Shirini, Farhad; Khaligh, Nader Ghaffari; Akbari-Dadamahaleh, Somayeh; Journal of Molecular Catalysis A: Chemical; vol. 365; (2012); p. 15 – 23;,
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As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 3236-48-4, name is trans-1,4-Cyclohexanedimethanol, molecular formula is C8H16O2, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. Recommanded Product: 3236-48-4

Step D: Preparation of ((lr,4r)-4-(Hydroxymethyl)cyclohexyl)methyl-3- fluorophenyl(phenyl)carbamate.; A suspension of 4-(dimethylamino)- 1 -((3 -fluorophenyl)(phenyl)carbamoyl)-pyridinium chloride (88.25 g, 237 mmol), (lr,4r)-cyclohexane-l,4-diyldimethanol (137 g, 950 mmol) and 4-dimethylaminopyridine (29.0 g, 237 mmol) in acetonitrile (1 L) was heated at 53 0C for 18 h. Upon cooling, the solvent was removed, and the residue was taken up in isopropyl acetate (500 mL) and 1 N HCl (500 mL), heated to suspend all solids, and then filtered through glass fiber filter paper to remove the insoluble bis-carbamate impurity. The aqueous filtrate was discarded, and the organic filtrate was washed with an additional 500 mL of 1 N HCl, followed by water (5 x 500 mL). Heptane (100 mL) was added to the organic phase, which was further washed with water (2 x 500 mL) and brine (100 mL), dried over MgSO4, and concentrated to dryness. The residue was taken up in isopropyl acetate (100 mL) and heptane (300 mL) was added. Crystals gradually formed over 1 h, forming a white precipitate, which was collected by filtration, rinsing with 25percent isopropyl acetate/heptane (100 mL). The filtrate was concentrated to dryness, and the hot residue was taken up in 25percent isopropyl acetate/heptane (100 mL) and filtered hot. As the filtrate cooled, more solids precipitated, which were collected by filtration and combined with the first crop. This material still contained about 5percent bis-carbamate by-product, which could not be readily removed by filtration. The solid was then taken up in dichloromethane (200 mL) and subjected to plug filtration over 1.6 kg of silica gel, eluting the remaining bis-carbamate with dichloromethane and the product with 20percent ethyl acetate/dichloromethane to provide the title compound as a white solid (71 g). LCMS m/z = 358.2 [M+H]+; 1H NMR (CDCl3, 400 MHz) delta 0.91-0.98 (m, 4H), 1.35-1.44 (m, IH), 1.54-1.60 (m, IH), 1.68-1.73 (m, 2H), 1.79-1.83 (m, 2H), 3.45 (d, 7= 6.4 Hz, 2H), 4.01 (d, J= 6.4 Hz, 2H), 6.91 (t, J= 7.6 Hz, IH), 7.04 (d, J = 8.6 Hz, 2H), 7.22-7.30 (m, 4H), 7.38 (t, J = 7.8 Hz, 2H).

With the rapid development of chemical substances, we look forward to future research findings about 3236-48-4.

Reference:
Patent; ARENA PHARMACEUTICALS, INC.; WO2009/117095; (2009); A1;,
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