Extracurricular laboratory: Synthetic route of 440-60-8

According to the analysis of related databases, 440-60-8, the application of this compound in the production field has become more and more popular.

Synthetic Route of 440-60-8, Adding some certain compound to certain chemical reactions, such as: 440-60-8, name is (Perfluorophenyl)methanol,molecular formula is C7H3F5O, 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 440-60-8.

General rocedure: 5.5 ml of aq. solutions of KBr (0.55 mol/dm3), 20 ml MeCN, TEMPO (0.12 g, 0.00077 mol), and 2,2,3-trifluoro-3-(1,1,2,2,3,3-hexafluoro-3-trifluoromethoxy-propoxy)-propan-1-ol (2a) (10 g, 0.0275 mol) were placed in the flask. 14% aq. NaOCl (48 ml) buffered by NaHCO3 (5.2 g) were added via the dropping funnel in 3 portions during two days of stirring in a room temperature (slight exothermic effect). The progress of reaction was monitored by 19F NMR spectroscopy. Then concentrated sulfuric acid followed by water was added. After extraction with diethyl ether, the organic phases were dried over magnesium sulfate. The solvent was evaporated to give a colorless liquid, which was distilled.

According to the analysis of related databases, 440-60-8, the application of this compound in the production field has become more and more popular.

Reference:
Article; Ignatowska, Jolanta; Shyshkov, Oleg; Zipplies, Tilman; Hintzer, Klaus; Roeschenthaler, Gerd-Volker; Journal of Fluorine Chemistry; vol. 141; (2012); p. 35 – 40;,
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A new synthetic route of 52244-70-9

Statistics shows that 52244-70-9 is playing an increasingly important role. we look forward to future research findings about 4-(4-Methoxyphenyl)-1-butanol.

Application of 52244-70-9, 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.52244-70-9, name is 4-(4-Methoxyphenyl)-1-butanol, molecular formula is C11H16O2, molecular weight is 180.24, as common compound, the synthetic route is as follows.

4-Methylphenylsulfonic acid 4-(4-methoxyphenyl)butyl ester (1). Pyridine (15 mL) was added drop wise to a cooled (0° C.) solution of 4-(4-methoxyphenyl)butanol (10.0 g, 0.055 mol) and p-toluenesulfonyl chloride (13.6 g, 0.072 mol) in dry chloroform (100 mL) under stirring. The reaction mixture was stirred overnight at room temperature. After this time, the reaction was quenched with 10percent HCl (300 mL) and extracted with chloroform. The organic fraction was washed with saturated NaHCO3, water and dried over magnesium sulfate. The solvent was removed under reduced pressure and the residue purified by flash chromatography (eluent: hexane/ ethyl acetate 15:1) to provide 12.9 g (66percent) of 1 as clear oil. 1H NMR (360 MHz, CDCl3) delta1.61 (m, 4H), 2.44 (s, 3H), 2.52 (m, 2H), 3.78 (s, 3H), 4.05 (m, 2H), 6.77 (d, 2H), 7.05 (d, 2H), 7.34 (d, 2H), 7.78 (d, 2H).

Statistics shows that 52244-70-9 is playing an increasingly important role. we look forward to future research findings about 4-(4-Methoxyphenyl)-1-butanol.

Reference:
Patent; CYFI, INC.; US2003/195160; (2003); A1;,
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Share a compound : 3562-73-0

At the same time, in my other blogs, there are other synthetic methods of this type of compound,3562-73-0, 1-(4-Biphenylyl)ethanol, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 3562-73-0, 1-(4-Biphenylyl)ethanol, 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, name: 1-(4-Biphenylyl)ethanol, blongs to alcohols-buliding-blocks compound. name: 1-(4-Biphenylyl)ethanol

h): Take a reaction tube and add sodium azide 49mg.1-[4-(1,1′-biphenyl)]ethanol 59.5 mg,400 uL of trifluoroacetic acid, 150 uL of methanesulfonic acid, 1.0 mL of n-hexane, and stirred at 50 C for 36 hours.After the reaction was completed, 10 mL of a sodium hydroxide solution was added to quench the reaction, and the mixture was extracted with ethyl acetate three times.The organic phase was washed with 5 mL of brine, and the organic phases were combined and separated by column chromatography to obtain 45.7 mg of p-phenylaniline.The yield was 90%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,3562-73-0, 1-(4-Biphenylyl)ethanol, and friends who are interested can also refer to it.

Reference:
Patent; Peking University; Jiao Ning; Liu Jianzhong; (27 pag.)CN109134267; (2019); A;,
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Introduction of a new synthetic route about tert-Butyl 2-hydroxyacetate

At the same time, in my other blogs, there are other synthetic methods of this type of compound,50595-15-8, tert-Butyl 2-hydroxyacetate, and friends who are interested can also refer to it.

Related Products of 50595-15-8, 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. 50595-15-8, name is tert-Butyl 2-hydroxyacetate. A new synthetic method of this compound is introduced below.

A suspension of 6-bromo-N-(4-fluoro-phenyl)-nicotinamide (0.112 g, 0.38 mmol), tert-butyl glycolate (0.1 g, 0.76 mmol), and potassium tert-butoxide (0.85 g, 0.76 mmol) in THF (10 mL) was heated in a sealed tube at 70° C. After 6 h the reaction mixture was diluted with ethyl acetate and washed with water bicarbonate and dried over sodium sulfate. Removal of the solvents provided a solid. Purification by reverse phase chromatography gave 0.010 g (8percent) of the titled product as a white solid; MS (EI) m/z 345.21 (M-H)-.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,50595-15-8, tert-Butyl 2-hydroxyacetate, and friends who are interested can also refer to it.

Reference:
Patent; Darwin Molecular Corporation; US6777432; (2004); B1;,
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Introduction of a new synthetic route about 3-Fluorobenzyl alcohol

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,456-47-3, its application will become more common.

Related Products of 456-47-3, 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. 456-47-3, name is 3-Fluorobenzyl alcohol. A new synthetic method of this compound is introduced below.

General procedure: Sodium hydride (60% in mineral oil, 0.04g, 1mmol) was added to a stirred solution of benzyl alcohol derivative (1mmol) in anhydrous N,N-dimethylformamide (3mL of DMF) at room temperature and stirring was continued for 1h. 2-Amino-3-chloropyrazine (10b, 0.13g, 1mmol) was added to the reaction mixture and the reaction mixture was stirred at 100C for 15h. After cooling, the solvent was evaporated and the residue was partitioned between water and dichloromethane. The organic layer was dried over sodium sulfate anhydrous, filtered, and concentrated. The residue was purified by column chromatography (SiO2, EA/n-Hex=1/5). 4.1.2.1 3-(3-Fluorobenzyloxy)pyrazin-2-amine (11e) (0027) Light orange solid, yield: 75.6%, 1H NMR (400MHz, DMSO-d6) delta=5.39 (2H, s, OCH2Ph), 6.36 (2H, br, NH2), 7.14 (1H, td, J=2.6Hz, 9.0Hz, ArH), 7.25 (1H, d, J=3.1Hz, ArH), 7.32 (1H, d, J=7.6Hz, ArH), 7.37-7.44 (2H, m, ArH), 7.49 (1H, d, J=3.1Hz, ArH).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,456-47-3, its application will become more common.

Reference:
Article; Park, Jung-eun; Elkamhawy, Ahmed; Hassan, Ahmed H.E.; Pae, Ae Nim; Lee, Jiyoun; Paik, Sora; Park, Beoung-Geon; Roh, Eun Joo; European Journal of Medicinal Chemistry; vol. 141; (2017); p. 322 – 334;,
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Sources of common compounds: Diethylene Glycol Monoethyl Ether

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,111-90-0, its application will become more common.

Synthetic Route of 111-90-0, 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 111-90-0 as follows.

EXAMPLE 6 11.2 g (0.083 mole) of diethylene glycol monoethyl ether was added dropwise to a mixture consisting of 1.6 g (0.042 mole) of sodium borohydride, 10 ml of xylene and 5 g (0.027 mole) of methyl caprate at 90 C. over two hours while agitating the mixture. Subsequently, the mixture was agitated at the same temperature for 2.5 hours. After cooling to room temperature, the mixture was neutralized with dilute sulfuric acid. As a result, n-decanol was obtained in 97% yield.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,111-90-0, its application will become more common.

Reference:
Patent; Kao Corporation; US5196601; (1993); A;,
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Extended knowledge of 4,4,5,5,5-Pentafluoropentan-1-ol

According to the analysis of related databases, 148043-73-6, the application of this compound in the production field has become more and more popular.

Synthetic Route of 148043-73-6, Adding some certain compound to certain chemical reactions, such as: 148043-73-6, name is 4,4,5,5,5-Pentafluoropentan-1-ol,molecular formula is C5H7F5O, 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 148043-73-6.

EXAMPLE 1 Into a 1L hastelloy C autoclave, pentafluoropentanol (C2F5(CH2)3OH, 519 g) and trifluoromethane sulfonic acid (20 g) were charged and stirred at 175C for 14 hours. The reactor pressure at that time was 0.7 MPa (gage pressure). After the reaction, the obtained crude liquid was subjected to liquid separation, and the organic phase was washed twice with water (50 ml) and dried over magnesium sulfate, followed by filtration to obtain a crude liquid. The conversion by the reaction was 75.7% as measured by gas chromatography (hereinafter referred to simply as GC). By distillation under reduced pressure, the desired following compound (I-1) (172 g) was obtained as a fraction of (60 to 61C)/1.4 kPa (absolute pressure). The GC purity was 99.9%. By the NMR analysis, formation of the following compound (I-1) was confirmed. Compound (I-1) : C2F5(CH2)3O(CH2)3C2F5.1HNMR (300.4MHz, CDCl3, TMS) delta (ppm) : 1.87 (m, 2H), 2.12 (m, 2H), 3.48 (m, 2H).19FNMR (282.7MHz, CDCl3, CFCl3) delta (ppm) : -86.1 (3F), -118.8(2F).

According to the analysis of related databases, 148043-73-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ASAHI GLASS COMPANY LTD.; EP1577284; (2005); A1;,
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Application of [1,1′-Biphenyl]-4-ylmethanol

According to the analysis of related databases, 3597-91-9, the application of this compound in the production field has become more and more popular.

Application of 3597-91-9, Adding some certain compound to certain chemical reactions, such as: 3597-91-9, name is [1,1′-Biphenyl]-4-ylmethanol,molecular formula is C13H12O, 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 3597-91-9.

A mixture of K2CO3 (1 mmol) and the catalyst (52 mg, ?3 mol% of Pd2+) in toluene (5 ml) was prepared in a two necked flask. The flask was evacuated and refilled with pure oxygen. To this solution, the alcohol (1 mmol, in 1 ml toluene) was injected and the resulting mixture was stirred at 80 C under an oxygen atmosphere. After completion of reaction, the reaction mixture was filtered off and the catalyst rinsed twice with CH2Cl2 (5 ml). The excess of solvent was removed under reduced pressure to give the corresponding carbonyl compounds.

According to the analysis of related databases, 3597-91-9, the application of this compound in the production field has become more and more popular.

Reference:
Article; Alizadeh; Khodaei; Kordestania; Beygzadeh; Journal of Molecular Catalysis A: Chemical; vol. 372; (2013); p. 167 – 174;,
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The important role of 30379-58-9

At the same time, in my other blogs, there are other synthetic methods of this type of compound,30379-58-9, Benzyl 2-hydroxyacetate, and friends who are interested can also refer to it.

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.30379-58-9, name is Benzyl 2-hydroxyacetate, molecular formula is C9H10O3, molecular weight is 166.17, as common compound, the synthetic route is as follows.Quality Control of Benzyl 2-hydroxyacetate

2-(Fluorenylmethoxycarbonyl)hydroxyacetic acid benzyl ester (657). To a solution of benzyl glycolate (6.0 g, 36.1 mmol) in CH2Cl2, cooled via ice-water bath, was added fluorenylmethoxy chloroformate (14 g, 1.5 equiv.) then diisopropylethylamine (9 mLs, 1.5 equiv.). After 1 hour, reaction mixture was poured into a saturated aqueaous solution of ammonium chloride and extracted with CH2Cl2, dried over Na2SO4 then concentrated in vacuo. The product was triturated from MeOH to obtain 2.2 g of 657 as a first crop of white solid. 2-(Fluorenylmethoxycarbonate) acetic acid (658). To a solution of 657 (2.2 g, 5.93 mmol) in tetrahydrofuran was added 5% Pd/C (220 mg). The resulting suspension was vigorously stirred under hydrogen atmosphere. After 90 min, the reaction mixture was filterred through Celite. The filtrate was poured into saturated aqueous NaHCO3 and washed twice with EtOAc. The aqueous layer was then acidified and the product extracted twice with CH2Cl2, dried over Na2SO4 and concentrated in vacuo to afford 1.46 g (88%) of 658 as a white solid. 2-(Fluorenylmethoxycarbonate) acetyl chloride (659), was prepared from 658 by the method used to prepare 643 to afford 659 as a crude product. (3S)-3-[(3S)-2-Oxo-3-(3,5-dichloro-4-hydroxybenzoyl)amino-5-(2-fluorenylmethoxycarbonate)acetyl-2,3,4,5-tetrahydro-1H-1,5-benzodiazepine-1-acetylamino]4-oxo-butyric acid tert-butyl ester semicarbazone (660), was synthesised from 600b, using 659, by methods used to prepare 604d from 600b to afford 453 mg of 660. (3S)-3-[(3S)-2-Oxo-3-(3,5-dichloro-4-hydroxybenzoyl)amino-5-(2-hydroxy)acetyl-2,3,4,5-tetrahydro-1H-1,5-benzodiazepine-1-acetylamino]4-oxo-butyric acid tert-butyl ester semicarbazone (661). A solution of 660 (423 mg) in MeOH:Et2NH (1:1, v/v) was stirred at ambient temperature.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,30379-58-9, Benzyl 2-hydroxyacetate, and friends who are interested can also refer to it.

Reference:
Patent; Vertex Pharmaceuticals Incorporated; US6204261; (2001); B1;,
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New downstream synthetic route of 33893-85-5

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,33893-85-5, its application will become more common.

Synthetic Route of 33893-85-5, 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 33893-85-5 as follows.

EXAMPLE 5 To acetic acid in which Ce (IV)/PFCP (50 mg, 0.027 mmole) and 200 mg of NaBrO3 were dispersed and dissolved, 1.0 mmole of 1,10-undecane diol and 1.0 mmole of 4-hydroxymethyl cyclohexanol were added, respectively. The reaction mixture was heated for three hours at 55 C. and the product was purified with a column chromatography to yield 154 mg (82% yield) of 10-undecane-1-ol and 93 mg (73% yield) of 4-hydroxymethyl cyclohexanone.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,33893-85-5, its application will become more common.

Reference:
Patent; E. I. Du Pont de Nemours and Company; US4617153; (1986); A;,
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