Category: alcohols-buliding-blocks

Application of 597-31-9 ,Some common heterocyclic compound, 597-31-9, molecular formula is C5H10O2, 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.

2,2-dimethyl-3-hydroxy – propionaldehyde(hydroxypivalaldehyde, Mitsubishi Gas Chemical Co., Ltd., purity 99.8%) 121.8gand 2-ethyl-2-hydroxymethyl- propane-1,3 – diol (trimethylolpropane, TokyoChemical industry reagent) 159.2 g, and benzene 1054g, granular Nafion (tradename “NR-50”, sigma-Aldrich reagent) 5.3g were housed in a 2 literround bottomed flask and at atmospheric pressure, water produced was withdrawnoutside the system using a Dean-Stark trap while azeotroping with benzene, andallowed to react until distillation of water ceased. This was filtered and thenrecrystallized by concentrating and cooling, to give 219.9g of crystal of 2-(5-ethyl-5-hydroxymethyl – [1,3] dioxan-2-yl) -2-methyl – propan-1-ol (hereinafter, referred to as “compound HTPA”.) as the sum of thegeometric isomers. Below, this synthetic reaction scheme was illustrated.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,597-31-9, its application will become more common.

Reference:
Patent; MITSUBISHI GAS CHEMICAL COMPANY INCORPORATED; OKAMOTO, ATSUSHI; SATO, HIDEYUKI; (21 pag.)JP2016/13986; (2016); A;,
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Application of 37729-18-3, Adding some certain compound to certain chemical reactions, such as: 37729-18-3, name is 2-([1,1′-Biphenyl]-4-yl)ethanol,molecular formula is C14H14O, 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 37729-18-3.

(1-3) Preparation of 4- (2-iodoethyl) biphenyl A solution of methanesulfonyl chloride (9.54 g) in tetrahydrofuran (150 ml) was added dropwise to a solution 2- (biphenyl-4-yl) ethanol (5.53 g) and triethylamine (10.18 g) in tetrahydrofuran (150 ml) at 5C under nitrogen atmosphere. After stirring at room temperature for 6 hours, the precipitated crystals were collected by filtration. The filtrate was concentrated under reduced pressure and the resultant residue was purified with silica-gel column chromatography using a 1 : 1 mixture of hexane/ethyl acetate to give methanesulfonate of 2- (BIPHENYL-4-YL) ethanol as a colorless liquid. Sodium iodide (6.23 g) was added to a solution of the methanesulfonate in 2-butanone (150 ml) and stirred at 70C for 3 hours. The precipitate was filtered off and 5% aqueous sodium thiosulfate (30 ml) was added to the filtrate and extracted with ethyl acetate. The ethyl acetate layer was washed with an aqueous saturated saline solution and then dried over anhydrous sodium sulfate. The solvent was distilled off, and the resultant residue was purified with silica-gel column chromatography using a 5: 1 mixture of hexane and ethyl acetate to give the title compound (7.31 g) as a colorless liquid.

According to the analysis of related databases, 37729-18-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Mitsubishi Pharma Corporation; WO2005/14525; (2005); A2;,
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Application of 624-95-3 ,Some common heterocyclic compound, 624-95-3, molecular formula is C6H14O, 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.

Typically, the dehydrogenation reactions were performedin a stainless steel autoclave equipped with an automatictemperature controller, a thermocouple, a magnetic stirrerand a pressure gauge. Taking catalytic dehydrogenationof 3,3-dimethyl-1-butanol as an example: 3,3-dimethyl-1-butanol (2 mmol), 6.6Cu-2Ni/gamma-Al2O3 (0.4 g), styrene(8 mmol) and mesitylene (2 mL) were added to the autoclave.After the autoclave was sealed, N2 was charged toreplace the air. Then, the autoclave was heated to 150 Cunder magnetic stirring within 20 min. After 24 h, the reactorwas cooled down to room temperature. The liquid reactionmixture was diluted and analyzed.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,624-95-3, its application will become more common.

Reference:
Article; Yang, Xiaomei; Fu, Xiaomin; Bu, Ningning; Han, Li; Wang, Jianfeng; Song, Chengying; Su, Yunlai; Zhou, Lipeng; Lu, Tianliang; Journal of the Iranian Chemical Society; vol. 14; 1; (2017); p. 111 – 119;,
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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. 2043-47-2, name is 1H,1H,2H,2H-Nonafluoro-1-hexanol. This compound has unique chemical properties. The synthetic route is as follows. Computed Properties of C6H5F9O

To a mixture, kept under stirring, of C4F3CH2CH2OH (200 g, 0.757 moles), tetrahydrofurane (350 ml) and cyclohexane (300 ml) at 250C, an aqueous solution of NaOH (400 ml, 50%) was added drop-wise. After stirring for 2 hours, benzyltriethyl ammonium chloride (25 g, 0.11 moles) as phase transfer catalyst, and then 1- bromopropane (170 g, 1.38 moles) were added. The reaction mixture was kept under stirring at 400C for 40 hours, then at 700C for 8 hours. The resulting mixture was poured into water and the organic phase thus obtained was washed two times with water. After removing the fraction having a low boiling point, the raw product was subjected to distillation at reduced pressure, ? thus obtaining 200 g of C4F9CH2CH2O (CH2) 2CH3 (yield 86%, boiling temp. 1470C, n 1.3255) . Spectrographic data confirm the obtained structure: GC/MS m/z at 305 (M- H)+, 377 (M-CH2CH3J+, 73 ( -CH2OCH2CH2CH3) +, 43 (- CH2CH2CHj) + ; for NMR data see Tables 1-2.

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, 2043-47-2, 1H,1H,2H,2H-Nonafluoro-1-hexanol.

Reference:
Patent; ALChiMI.A. S.r.l.; WO2009/133575; (2009); A1;,
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Adding a certain compound to certain chemical reactions, such as: 2240-88-2, 3,3,3-Trifluoropropan-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, category: alcohols-buliding-blocks, blongs to alcohols-buliding-blocks compound. category: alcohols-buliding-blocks

Example 114 2-[3-(2-Fluorobenzyl)-1H-pyrazolo[4,3-b]pyridin-1-yl]-5,5-dimethyl-4-(3,3,3-trifluoropropoxy)-5,7-dihydro-6H-pyrrolo[2,3-d]pyrimidin-6-one Under argon, 57 mg (0.22 mmol) of triphenyl phosphine was dissolved in 1.5 ml THF, 43 mul (0.22 mmol) of diisopropyl azodicarboxylate and 25 mg (0.22 mmol) of 3,3,3-trifluoropropan-1-ol were added and it was stirred for 10 min. Then a suspension of 80 mg of example 109 in 0.5 ml DMF, which had been treated for 3 min in the ultrasonic bath, was added and the reaction mixture was stirred overnight at RT (solution). A further 57 mg (0.22 mmol) of triphenyl phosphine was added, the mixture was treated for 10 min in the ultrasonic bath, then a further 43 mul (0.22 mmol) of diisopropyl azodicarboxylate was added and it was stirred overnight. Then a further 25 mg (0.22 mmol) of 3,3,3-trifluoropropan-1-ol and 57 mg (0.22 mmol) of triphenyl phosphine were added, the reaction mixture was treated for 10 min in the ultrasonic bath, then 43 mul (0.22 mmol) of diisopropyl azodicarboxylate was added and it was stirred for another night at RT. The reaction mixture was purified by preparative HPLC (Reprosil C18, gradient of acetonitrile/0.01percent aq. formic acid). Yield: 37 mg (37percent of theor.) LC-MS (method 1): Rt=1.21 min; MS (ESIpos): m/z=501 [M+H]+ 1H-NMR (400 MHz, DMSO-d6): delta [ppm]=1.35 (s, 6H), 2.92 (qt, 2H), 4.79 (t, 2H), 5.87 (s, 2H), 7.11-7.27 (m, 3H), 7.32-7.41 (m, 1H), 7.45 (dd, 1H), 8.68 (dd, 1H), 8.86 (dd, 1H), 11.45 (s, 1H).

The synthetic route of 2240-88-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER INTELLECTUAL PROPERTY GMBH; FOLLMANN, Markus; STASCH, Johannes-Peter; REDLICH, Gorden; GRIEBENOW, Nils; LANG, Dieter; WUNDER, Frank; HUeBSCH, Walter; LINDNER, Niels; VAKALOPOULOS, Alexandros; TERSTEEGEN, Adrian; US2013/338137; (2013); A1;,
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Electric Literature of 4139-61-1, 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. 4139-61-1, name is 6-Bromo-4-hydroxycoumarin. A new synthetic method of this compound is introduced below.

Step one: the 6 – bromo -4 – hydroxy coumarin (1 mmol) with triethylamine (1.5 mmol) dissolved in 10 ml dichloromethane after, cold water bath cooling, trifluoromethyl sulfonic acid anhydride (1.5 mmol) is added slowly dropping in the reaction system, the reaction 3 hours later, and steaming and to remove the solvent, after concentrating column separation (petroleum ether and ethyl acetate to the volume proportion 4:1) to obtain 6 – bromo -4 – trifluoromethanesulfonic acid ester – coumarin.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,4139-61-1, its application will become more common.

Reference:
Patent; Henan University of Technology; Wang Hongyan; Wei Xuning; Liu Yu; Guo Tao; Lin Xiangbin; Kong Linghui; (33 pag.)CN107629050; (2018); A;,
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Application of 612-16-8 , The common heterocyclic compound, 612-16-8, name is (2-Methoxyphenyl)methanol, molecular formula is C8H10O2, 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: Reactions were performed in a magnetically stirred round bottomed flask fitted with acondenser and placed in a temperature controlled oil bath. 1,2-Diamine (2 mmol)was added to alcohol (3 mmol) and the reaction mixture was allowed to stir at 135C in an open (air) atmosphere. After disappearance of the diamine (reaction was monitored by TLC)or after the appropriate time, the reaction mixture was cooled to roomtemperature. The crude residue was further purified by column chromatography using silica gel (100-200 mesh) to afford pure products. All the products wereidentified on the basis of NMR and mass spectral data

The synthetic route of 612-16-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Marri, Mahender Reddy; Peraka, Swamy; Macharla, Arun Kumar; Mameda, Naresh; Kodumuri, Srujana; Nama, Narender; Tetrahedron Letters; vol. 55; 48; (2014); p. 6520 – 6525;,
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Application of 2566-44-1, 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.2566-44-1, name is 2-Cyclopropylethanol, molecular formula is C5H10O, molecular weight is 86.13, as common compound, the synthetic route is as follows.

Take a single-necked flask and add 2-cyclopropylethanol (2.4g, 28mmol), DMF (30mL) in sequence, cool to 0 C, add sodium hydrogen (1.3g, 33mmol, 60% by mass), and stir the reaction mixture at room temperature for 20min Add 3- (benzyloxy) 2-bromo-6-iodopyridine (10g, 25.6mmol), heat to 100 C and continue stirring for 12h.Post-treatment: add water (50 mL) to quench the reaction, extract with ethyl acetate (20 mL × 3), combine the organic phases, wash the organic phase with saturated brine (50 mL × 3), dry over anhydrous sodium sulfate, filter, and concentrate under reduced pressure The filtrate and the residue were separated by silica gel column chromatography (PE / EA (V / V) = 2/1) to obtain the title compound as a colorless oil (6.8 g, 17 mmol, 67%).

Statistics shows that 2566-44-1 is playing an increasingly important role. we look forward to future research findings about 2-Cyclopropylethanol.

Reference:
Patent; Guangdong Dongyangguang Pharmaceutical Co., Ltd.; Huang Jianzhou; Ren Qingyun; Xiong Jinfeng; Liu Yang; Yu Fangcai; Liu Weishun; Wang Yifeng; Zhang Yingjun; (104 pag.)CN110903284; (2020); A;,
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Related Products of 764-48-7, 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 764-48-7, name is Ethylene Glycol Vinyl Ether. This compound has unique chemical properties. The synthetic route is as follows.

General procedure: A dry and argon-flushed 10 mL Schlenk tube, equipped with a stirring bar and septum, wascharged with 2-(vinyloxy)ethanol (5, 132 mg, 1.50 mmol, 1.50 equiv) in Et2O (1.5 mL). Then,iPrMgBr (1.55 mmol, 1.55 equiv) was added dropwise at 25 C. After 5 min of stirring,Sc(OTf)3 (49.2 mg, 0.10 mmol, 0.10 equiv) and aldehyde 6 (1.00 mmol, 1.00 equiv) weresuccessively added and the reaction mixture was stirred at 40 C for the given time. After afull conversion was detected by GC-analysis, sat. aq. NH4Cl (15 mL) was added and theaqueous layer was extracted with EtOAc (3 x 15 mL). The combined organic layers weredried over Na2SO4, filtered and solvent was removed under reduced pressure. Purification viacolumn chromatography (SiO2) afforded expected products 4.

According to the analysis of related databases, 764-48-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Quinio, Pauline; Kohout, Laura; Roman, Daniela Sustac; Gaar, Jakob; Karaghiosoff, Konstantin; Knochel, Paul; Synlett; vol. 27; 11; (2016); p. 1715 – 1719;,
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Synthetic Route of 346-06-5, 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 346-06-5, name is (2-(Trifluoromethyl)phenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows.

Example 99; 5-(2-Trifluoromethylbenzyloxy)-quinazoline-2,4-diamine; [00297] Step 1; 2- (Trifluoromethyl)benzyl alcohol(1.15 g; 6.3 mmol) was added to a cooled (0 °C) slurry of sodium hydride (243.7 mg; 6 mmol) in dimethylformamide under nitrogen atmosphere. The reaction mixture was slowly warmed to room temperature, stirred for 45 min.. The reaction mixture was then added to a cooled (0 °C) solution of 2,6-difluorobenzonitrile in dimethylformamide , stirred for 3 hours at room temperature. The reaction mixture was poured on crushed ice-water, stirred, filtered, washed with water and dried to afford 1.39 grams of 2-fluoro-6-(2-trifluoro- methylphenyl-methoxy) benzonitrile as a white solid.

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 346-06-5, (2-(Trifluoromethyl)phenyl)methanol.

Reference:
Patent; DECODE CHEMISTRY, INC.; SINGH, Jasbir; GURNEY, Mark E.; WO2005/123724; (2005); A1;,
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