Month: July 2021

Electric Literature of 96-35-5, 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. 96-35-5, name is Methyl 2-hydroxyacetate, molecular formula is C3H6O3, 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: Hydrogenation of Other Ester Compounds Catalyzed by Synthetic Preparation of Bipyridine Tetradshed Ruthenium Complex 5 The results are shown in Table 2:Table 2 Hydrogenation of other ester compounds a; A Reaction conditions: S / C = 1000,3.0 mmol Substrate, 3.0 mumol 5, 3.0 mL lPrOH, 0.3 mmol NaOMe, 5 MPa H2, 25 C; D 100 C.

According to the analysis of related databases, 96-35-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Nankai University; Zhou, Qilin; Li, Wei; Xie, Jianhua; Wang, Lixin; (22 pag.)CN103980317; (2017); B;,
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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 15258-73-8, name is (2,6-Dichlorophenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows. Safety of (2,6-Dichlorophenyl)methanol

[Example 10] Synthesis of sodium 2,6-dichlorobenzyloxymethyl trifluoroborate To the mixture of sodium hydride (61 %, 180 mg, 4.5 mmol) and tetrahydrofuran (6 ml), 2,6-dichlorobenzyl alcohol (740 mg, 4.2 mmol) was added at 0C (an outer temperature), and the obtained reaction mixture was stirred at room temperature for 1 hour. To the reaction mixture, 2-(bromomethyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (92%, 500 mg, 2.1 mmol) synthesised in Production Example 2 and dissolved in tetrahydrofuran (4 ml) was added at 0C (an outer temperature), and the obtained mixture was stirred at 30C (an outer temperature) overnight. After cooling the reaction mixture to 0C (an outer temperature), sodium hydrogen fluoride (590 mg, 4.5 mmol) was added to the reaction mixture at the same temperature, followed by the dropwise addition of water (8 ml) at the same temperature. After stirring the reaction mixture for 30 minutes at room temperature, the solvents were evaporated under reduced pressure. Acetone (40 ml) was added to the obtained residue, followed by filtration. The solvents were evaporated under reduced pressure from the filtrate, and then the obtained residue was washed with diethyl ether, thereby obtaining the entitled compound (460 mg, 78%). 1H-NMR Spectrum (DMSO-d6) delta(ppm): 2.61(2H, q, J=5.4Hz), 4.46(2H, s), 7.30-7.35(1H, m), 7.44(2H, d, J=8.0Hz)

With the rapid development of chemical substances, we look forward to future research findings about 15258-73-8.

Reference:
Patent; Eisai R&D Management Co., Ltd.; EP2062901; (2009); A1;,
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Reference of 2215-78-3, 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. 2215-78-3, name is (4-Phenoxyphenyl)methanol. A new synthetic method of this compound is introduced below.

To a solution of (4-phenoxy-phenyl)-methanol (408 mg, 2.04 mmol) in carbon tetrachloride (8.2 mL) was added triphenylphosphine (642 mg, 2.45 mmol) under nitrogen atmosphere at room temperature, and the reaction solution was stirred under reflux for 7 hours and 40 minutes. The reaction mixture was cooled to room temperature and concentrated under a reduced pressure. The residue was purified by silica gel column chromatography (heptane:ethyl acetate=10:1) to obtain the title compound (409 mg, 92%). 1H-NMR Spectrum (DMSO-d6) delta (ppm): 4.76 (2H, s), 6.98-7.05 (4H, m), 7.15-7.19 (1H, m), 7.39-7.46 (4H, m).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2215-78-3, (4-Phenoxyphenyl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; Eisai R&D Management Co., Ltd.; US2007/105904; (2007); 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. 1805-32-9, name is 3,4-Dichlorobenzyl alcohol. This compound has unique chemical properties. The synthetic route is as follows. Product Details of 1805-32-9

Examples 204-206 were prepared according to the method described below: 6′-[(3R)-3-{[tert-Butyl(dimethyl)silyl]oxy}pyrrolidin-1-yl]-2-oxo-2H-1,3′-bipyridin-4-yl 4-bromobenzenesulfonate from Preparation 47 (197 mg, 0.324 mmol), the appropriate benzyl alcohol (0.982 mmol) and potassium hydroxide (55 mg) in DMSO (3 ml) were heated at 130 C. under nitrogen for 1 hour then allowed to stand at r.t. overnight. The reactions were diluted with methanol (3 ml) and passed down a SCX column, washed with methanol and the product eluted with 2M NH3 in methanol, evapourated to dryness. The residue was chromatographed on Biotage 12×150 mm silica column eluting with DCM/MeOH/NH3 98/2/0 to 93/7/1. Solvent removed in vacuo to give the title compound as solids. 204 LC-MS RT = 1.20 min m/z (APCI & ESI) 432 [MH+](2 min run)

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, 1805-32-9, 3,4-Dichlorobenzyl alcohol.

Reference:
Patent; Pfizer Inc; US2008/85884; (2008); A1;,
Alcohol – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 17849-38-6, 2-Chlorobenzyl alcohol, 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, Quality Control of 2-Chlorobenzyl alcohol, blongs to alcohols-buliding-blocks compound. Quality Control of 2-Chlorobenzyl alcohol

General procedure: A mixture of the substrate (1 mmol), hexamethyldisilazane (0.70 mmol), and/or 3,4-dihydro-2H-pyran (1.4 mmol) and BiPy(SO3H)2(HSO4)2 (10 mg, 1.95 mol%) in CH3CN(3 mL) and/or CH2Cl2 (3 mL) was stirred at room temperature. The progress of thereaction was monitored by TLC (n-hexane: EtOAc; 10:1) and/or GC. After completion ofthe reaction, the mixture was filtered to separate the solid catalyst. Then the solution wasfiltered through a silica gel pad and washed with CH3CN (2 × 3 mL) and/or CH2Cl2 (2 ×3 mL). Evaporation of the solvent gave the desired products in high purity.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,17849-38-6, 2-Chlorobenzyl alcohol, and friends who are interested can also refer to it.

Reference:
Article; Shirini, Farhad; Abedini, Masoumeh; Mahmoodi, Nosratollah; Biglari, Mohammad; Safarpoor Nikoo Langrudi, Mohaddeseh; Phosphorus, Sulfur and Silicon and the Related Elements; vol. 190; 11; (2015); p. 1912 – 1921;,
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Synthetic Route of 637031-88-0, 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.637031-88-0, name is 3,3-Difluorocyclobutanol, molecular formula is C4H6F2O, molecular weight is 108.09, as common compound, the synthetic route is as follows.

To a 10-mL Schlenk tube were added Example 8f (240 mg, 0.8 mmol), Example lj (130 mg, 1.2 mmol), K2C03 (221 mg, 1.6 mmol) and DMF (4 mL). The tube was sealed and heated at 80C for 16 hours. The reaction was cooled to room temperature. Water (10 mL) was added, the mixture was extracted by EtOAc (10 mL*3). The combined organic phase was washed with brine, dried over Na2SO4, filtrated and concentrated under reduced pressure to give the crude product which was further purified by silica gel chromatography to give the pure product Example 8g (92 mg, yield 30%) as a white solid. ?H NMR (400 IVIHz, Chloroform-d) 7.36 (d, J 8.6 Hz, 1H), 6.86 (d, J 8.6 Hz, 1H), 4.77 (d, J= 9.3 Hz, 1H), 4.39-4.33 (m, 2H),4.28-4.23 (m, 2H), 3.13 (ddt, J 18.9, 12.3, 6.5 Hz, 2H), 2.94-2.81 (m, 2H).

Statistics shows that 637031-88-0 is playing an increasingly important role. we look forward to future research findings about 3,3-Difluorocyclobutanol.

Reference:
Patent; FRONTHERA U.S. PHARMACEUTICALS LLC; JIN, Bohan; DONG, Qing; HUNG, Gene; (151 pag.)WO2018/31680; (2018); A1;,
Alcohol – Wikipedia,
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Electric Literature of 115652-52-3, 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. 115652-52-3, name is (1-Aminocyclopropyl)methanol hydrochloride. A new synthetic method of this compound is introduced below.

Intermediate: 5-((5-((3′-(3-bromopropoxy)-2′-chloro-2-methyl-[1,1′-biphenyl]-3-yl)methoxy)-4-chloro-2-(((1-(hydroxymethyl)cyclopropyl)amino)methyl)phenoxy)methyl)nicotinonitrile To a solution of 5-((5-((3′-(3-bromopropoxy)-2′-chloro-2-methyl-[1,1′-biphenyl]-3-yl)methoxy)-4-chloro-2-formylphenoxy)methyl)nicotinonitrile (20 mg, 0.031 mmol) in a mixture of 1,2-dichloroethanel (0.8 mL) and EtOH (0.5 mL) was added (1-aminocyclopropyl)methanol, HCl (12 mg, 0.097 mmol), acetic acid (3 muL, 0.052 mmol), and 4 A mol sieves. The reaction was flushed briefly with N2, capped, stirred at room temp for 90 min, then treated dropwise (over 1 h) with sodium cyanoborohydride, 1.0M in THF (65 muL, 0.065 mmol) and stirred at room temp for 18 h. Additional sodium cyanoborohydride (15 mulit) was added dropwise and the reaction was stirred at room temp for 1 h. N,N-diisopropylethylamine (15 muL) was added and the reaction stirred at room temp for 1.5 h. The solvent was removed under a gentle stream of N2 to give the title compound that was used “as is” without purification in subsequent reactions. LC/MS Condition A: ret time 1.18 min; m/e=710(M+H)+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,115652-52-3, (1-Aminocyclopropyl)methanol hydrochloride, and friends who are interested can also refer to it.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; YEUNG, KAP-SUN; Connolly, Timothy P.; Frennesson, David B.; Grant-Young, Katharine A.; Hewawasam, Piyasena; Langley, David R.; Meng, Zhaoxing; Mull, Eric; Parcella, Kyle E.; Saulnier, Mark George; Sun, Li-Qiang; Wang, Alan Xiangdong; Xu, Ningning; Zhu, Juliang; Scola, Paul Michael; (511 pag.)US2017/107202; (2017); A1;,
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Electric Literature of 480449-99-8, 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. 480449-99-8, name is Benzyl 3-hydroxycyclobutanecarboxylate. A new synthetic method of this compound is introduced below.

REFERENTIAL EXAMPLE 152 3-Hydroxycyclobutanecarboxylic acid: 10% Palladium on carbon (108 mg) was added to a solution of the compound (706 mg) obtained in Referential Example 151 in ethanol (10 ml), and the mixture was stirred at room temperature for 2 hours in a hydrogen atmosphere. After the catalyst was removed by filtration through Celite, the filtrate was concentrated under reduced pressure to obtain the title compound (399 mg). 1H-NMR (CD3OD) delta: 2.00-2.21(2H,m), 2.41-2.61(3H,m), 4.01-4.13(1H,m).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,480449-99-8, its application will become more common.

Reference:
Patent; DAIICHI PHARMACEUTICAL CO., LTD.; US2005/20645; (2005); A1;,
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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. 6351-10-6, name is 2,3-Dihydro-1H-inden-1-ol, the common compound, a new synthetic route is introduced below. name: 2,3-Dihydro-1H-inden-1-ol

General procedure: A mixture of alcohol or phenol (1 mmol), DHP (1.2-1.4 mmol), and MNPs-PSA (5 mg, 0.95 mol%) was stirred at room temperature in dry CH2Cl2 (2 mL), and the progress of the reaction was monitored by TLC. After completion of the reaction, catalyst was separated by an external magnet and washed with CH2Cl2. Then, the pure product was isolated by passing of the reaction mixture through a short column using n-hexane and ethyl acetate (9:1) as eluent.

The synthetic route of 6351-10-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Rostami, Amin; Tahmasbi, Bahman; Abedi, Fatemeh; Research on Chemical Intermediates; vol. 42; 4; (2016); p. 3689 – 3701;,
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Synthetic Route of 100-37-8, 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 100-37-8 as follows.

General procedure: To a solution of phenol (1 equiv), triphenylphosphine (1.3equiv) and 2-(diethylamino)ethanol (1.3 equiv) in THF wasadded diisopropyl azodicarboxylate (DIAD, 1.3 equiv) atambient temperature. After being stirred at ambient temperatureuntil no starting material could be observed byTLC, the reaction mixture was quenched with H2O anddiluted with EtOAc. The organic layer was washed withwater and brine, dried over MgSO4, and concentrated invacuo. Purification of the residue via flash column chromatographyon silica gel afforded the titled compound.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,100-37-8, its application will become more common.

Reference:
Article; Kim, Seok-Ho; Han, Young Taek; Archives of Pharmacal Research; vol. 38; 11; (2015); p. 1952 – 1962;,
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