Month: March 2021

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. 14002-73-4, name is Ethyl 3-hydroxy-2,2-dimethylpropanoate, molecular formula is C7H14O3, 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. category: alcohols-buliding-blocks

A solution of distilled sulfuryl chloride (0.55 mL, 7.5 mmol) in Et2O (10 mL) was cooled to -78 C. under an atmosphere of argon. A solution of ethyl 3-hydroxy-2,2-dimethylpropanoate (2a) (1.0 g, 6.8 mmol) and pyridine (0.55 mL, 6.8 mmol) in Et2O (1.0 mL) was then added dropwise over 1 h via a syringe. The syringe was rinsed with Et2O (3¡Á1 mL), each rinse being added to the reaction mixture. The acetone/CO2 bath was removed, and the mixture was allowed to warm to room temperature, then stirred at room temperature for 4 h. TLC analysis (EtOAc/hexanes; 3:7) did not indicate that the reaction was complete. The mixture was re-cooled to -78 C. and more SO2Cl2 (0.11 mL) was added, and the mixture allowed to warm to room temperature and stirred for an additional 2 h. The mixture was filtered and the filtrate was concentrated under vacuum to give the product (yield assumed quantitative). 1H NMR (300 MHz, CDCl3): delta 4.50 (s, 2H), 4.19 (q, J=6.9 Hz, 2H), 1.31 (s, 6H), 1.28 (t, J=6.9 Hz, 3H)

With the rapid development of chemical substances, we look forward to future research findings about 14002-73-4.

Reference:
Patent; ARIXA PHARMACEUTICALS, INC.; Gordon, Eric M.; Freund, John; Gallop, Mark A.; Duncton, Matthew Alexander James; (117 pag.)US10085999; (2018); B1;,
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Electric Literature of 44565-27-7 ,Some common heterocyclic compound, 44565-27-7, molecular formula is C5H13NO, 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-Nitrobenzaldehyde (7.33 g, 48.5 mmol) and 4-amino-2-methylbutanol (5.00 g, 48.5 mmol) where dissolved in toluene (50 ml) and heated to reflux for two hours with Dean Stark dehydration apparatus. After allowed to cool, the solvent was evaporated under reduced pressure. The obtained concentrate was dissolved in methanol (100 ml), added with sodium borohydride (2.75 g, 72.8 mmol) under ice cooled condition and stirred at the same temperature for two hours. The reaction mixture was further stirred at room temperature for two hours, adjusted to pH 4 by adding 1N hydrochloric acid, and the solvent was evaporated under reduced pressure. Water (30 ml) was added to dissolve the concentrate alter extracted with ethyl acetate, pH was adjusted to 8 by added a saturated sodium hydrogen carbonate aqueous solution and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and the solvent was evaporated under reduced pressure to obtain 2-methyl-4-(2-nitrobenzylamino)butanol (11.12 g). Yield: 96% Physical properties: nD 1.5372 (24C)

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. 44565-27-7, 4-Amino-2-methylbutan-1-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Nihon Nohyaku CO., LTD.; EP2085392; (2009); A1;,
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Electric Literature of 627-30-5, 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 627-30-5, name is 3-Chloropropan-1-ol. This compound has unique chemical properties. The synthetic route is as follows.

IMB105 (1.0g, 2.5mmol), 2-bromoethanol (0.22mL, 3.0mmol) or 3-chloropropanol (0.25mL, 3.0mmol), and PPh3 (1.3g, 5.0mmol) were added to dried THF (20mL) under Ar2. The obtained solution was cooled on an ice-water bath. DEAD (2.0mL, 4.25mmol, 40% in tulene) was added to the solution, and the reaction mixture was then allowed to warm to room temperature and stirred for 12h. The solvent was removed in vacuo, and the obtained residue was extracted into ethyl acetate (100mL). The organic layer was washed consecutively with water (50mL), brine (50mL), dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified on silica gel using Petroleumether (60-90C)/ethyl acetate in different proportions to afford 5 or 6.

According to the analysis of related databases, 627-30-5, the application of this compound in the production field has become more and more popular.

Reference:
Article; Gu, Yuxi; Hu, Laixing; Liu, Yonghua; Sun, lianqi; Wu, Yanbin; European Journal of Medicinal Chemistry; vol. 191; (2020);,
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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. 111-46-6, name is 2,2′-Oxybis(ethan-1-ol), the common compound, a new synthetic route is introduced below. SDS of cas: 111-46-6

Diethylene glycol (7.0 g, 66.0 mmol) was dissolved in 10 mL of dichloromethane solution, Et3N (13.3 g, 132.2 mmol) was added, and TsCl (15.1 g, 79.1 mmol) in dichloromethane was added dropwise on ice. .After the completion of the dropwise addition, the mixture was transferred to room temperature and stirred overnight.After adjusting the pH of the solution to 7 with 6 mol/L HCl, 10 mL of water was added, and the mixture was extracted three times with 30 mL of dichloromethane, and the organic phases were combined and dried over anhydrous sodium sulfate.Column chromatography (EA) gave 10 g of a yellow liquid product, yield 60%.

The synthetic route of 111-46-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zhejiang University of Technology; Zhang Xingxian; He Kailun; Wang Wenbing; Wang Xiaoju; Zheng Xiaoliang; (23 pag.)CN110204532; (2019); A;,
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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. 52059-53-7, name is 2-(3-Fluorophenyl)ethanol. This compound has unique chemical properties. The synthetic route is as follows. Recommanded Product: 2-(3-Fluorophenyl)ethanol

Dess-Martin periodinane (16.781 mmol, 1 .2 eq) is added to a solution of 3-fluorophenethyl alcohol (13.984 mmol, 1 eq) in DCM (32 mL). The resulting reaction mixture is stirred at RT for 4 h. The solvent is then partially evaporated, and the residue filtered through a short pad of Celite. The filtrate is concentrated under reduced pressure and the residue purified by FC (EtOAc/heptane, 5:95). Crude 2-(3-fluorophenyl)acetaldehyde is obtained as a colorless oil (2.58 g). The compound is used in the next step without further purification. 1H NMR (CDCI3): ?9.77 (t, J = 3.0 Hz, 1 H), 7.33 (m, 1 H), 6.98 (m, 3 H), 3.69 (d, J = 3.0 Hz, 2 H).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 52059-53-7, 2-(3-Fluorophenyl)ethanol.

Reference:
Patent; ACTELION PHARMACEUTICALS LTD; BOSS, Christoph; BROTSCHI, Christine; HEIDMANN, Bibia; SIFFERLEN, Thierry; WILLIAMS, Jodi T.; WO2012/85852; (2012); A1;,
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Reference of 597-31-9, Adding some certain compound to certain chemical reactions, such as: 597-31-9, name is 3-Hydroxy-2,2-dimethylpropanal,molecular formula is C5H10O2, 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 597-31-9.

The hydrogenation feed as described in example 1 was used.Catalyst UsedThe catalyst described in example 1 was used, but 3¡Á3 mm pellets were produced.The catalyst comprised 55% of CuO and 45% by weight of Ak2O3, had a specific surface area (BET) of 95 m2/g, an Hg porosity of 0.38 ml/g and a tapped density of 1042 g/l.HydrogenationThe hydrogenation input was passed through the reactor in the downflow mode at an H2 pressure of 40 bar. The temperature in the upper half of the reactor was 96 C., and that in the lower half was 106 C. The WHSV was 0.37 kg of HPA/(kgcat*h). Together with the liquid input, about 110 mol % of H2 (based on methyolalkanals used) were metered in, corresponding to a hydrogen/starting material molar ratio of 1:1. Part of the hydrogenation output was mixed back into the input (recycle mode). The ratio of recycle to input was 16:1. A mean conversion of 95.9% at a mean pH of 8.3 was achieved over a number of days; Example 3 was repeated under the conditions indicated but the amount of hydrogen was doubled to a hydrogen/starting material molar ratio of 2.2 and the temperature was reduced to 93 C. in the upper half of the reactor and 103 C. in the lower half of the reactor. A mean conversion of 95.6% at a pH of 8.4 was achieved.

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. 597-31-9, 3-Hydroxy-2,2-dimethylpropanal, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BASF Aktiengesellschaft; US2007/282135; (2007); A1;,
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Electric Literature of 84851-56-9 ,Some common heterocyclic compound, 84851-56-9, molecular formula is C10H12O3, 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 methyl-4-(l-hydroxyethyl)benzoate (2.00 g, 11.10 mmol) in a mixture of THF (20 mL) and MeOH (10 mL) was added 1 M KOH (13.32 mL, 13.32 mmol). After stirring at room temperature overnight, the solution was diluted with 2 N HCl and extracted with EtOAc (4x). The combined organic layers were dried (MgSO4) and evaporated to give 4-(l-hydroxyethyl)benzoic acid as a colorless solid. 1H NMR (DMSO-dzeta, 600 MHz) delta 7.86 (d, J = 8.6 Hz, 2H), 7.43 (d, J = 8.3 Hz, 2H), 4.75 (q, J = 6.5 Hz, IH), 1.30 (d, J = 6.6 Hz, 3H). MS: cal’d 167 (MH+), exp 167 (MH+).

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. 84851-56-9, Methyl 4-(1-hydroxyethyl)benzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK & CO., INC.; WO2008/10985; (2008); A2;,
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Application of 1777-82-8, 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. 1777-82-8, name is (2,4-Dichlorophenyl)methanol, molecular formula is C7H6Cl2O, 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.

General procedure: Catalytic experiments were carried out in a 5-mL test tube. In a typical procedure, to 1 mmol benzyl alcohol in 1 ml solvent, 2 mol% (0.02 g) of gamma-Fe2O3-MoO2L and 2 mmolof 30 % H2O2 was added. The reaction mixture was stirred for 3 h at 80 C. The reaction products were monitored byTLC or GC. After completion of the reaction, the mixture was diluted with EtOAc. The catalyst was separated by an external magnet, washed with EtOAc, dried and reused for a consecutive run under the same reaction conditions. Evaporation of the solvent from the filtrate under reduced pressure gave the crude products, which were then purified by chromatography on silica gel eluted with n-hexane/EtOAc (2:1).

According to the analysis of related databases, 1777-82-8, the application of this compound in the production field has become more and more popular.

Reference:
Article; Saeednia; Ardakani, M. Hatefi; Parizi, Z. Pakdin; Hafshejani, M. Tavakoli; Transition Metal Chemistry; vol. 41; 7; (2016); p. 767 – 774;,
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Adding a certain compound to certain chemical reactions, such as: 30379-58-9, Benzyl 2-hydroxyacetate, 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, 30379-58-9, blongs to alcohols-buliding-blocks compound. Computed Properties of C9H10O3

To a mixture of 78 (0.14 g, 2.51 mmol) and CS2C03 (0.16 g, 5.0 mmol) in DMF (2 mL) was added benzyl glycolate (0.05g, 3 mmol), and resulting mixture was stirred at 70 C for 8 h. DMF was removed in vacuo and residue was purified by flash chromatography on silica gel eluting with 10%MeOH/DCM to afford O.lg (62%) 79: MS (ES+) m/z 640 (M + H)+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,30379-58-9, its application will become more common.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; WO2005/121145; (2005); A2;,
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Application of 1124-63-6 ,Some common heterocyclic compound, 1124-63-6, molecular formula is C9H18O, 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.

3-Cyclohexylpropanal To a solution of commercially available 3-cyclohexylpropanol (45.5 g, 0.32 mol) in CH2C12 (1000 mL) was added PCC (103.5 g, 0.48 mol), Celite 545 (50 g) and stirred at room temperature for 3 h. The reaction mixture was diluted with ethyl ether (1000 mL), stirred at rt for 1 h, before it was filtered through Celite and silica gel (1 : 1) pad. The filtrate was concentrated to give crude residue. Crude product was purified by silica gel flash chromatography (0-30% EtOAc/hexanes) to give the title compound as oil (50.7 g), which contained residual hexanes as judged by NMR analysis. lH NMR (300 MHz, CDCb) delta 0.83 – 0.98 (m, 3 H), 1.15 – 1.31 (m, 4 H), 1.49 – 1.56 (m, 2 H), 1.61 – 1.73 (m, 4 H), 2.41 – 2.46 (m, 2 H), 9.77 (s, 1 H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,1124-63-6, its application will become more common.

Reference:
Patent; RESEARCH TRIANGLE INSTITUTE; RUNYON, Scott, P.; MAITRA, Rangan; NARAYANAN, Sanju; THOMAS, James, Barnwell; REHDER, Kenneth, S.; OLEPU, Srinivas; (194 pag.)WO2017/100558; (2017); A1;,
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