Month: June 2021

Application of 64372-62-9, 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. 64372-62-9, name is 2-Chloro-5-(trifluoromethyl)benzyl alcohol. A new synthetic method of this compound is introduced below.

A 3 M K2CO3 solution is prepared by adding solid K2CO3 (31 g, 0.22 mol) to water (100 mL). Cooling is applied to keep the solution at 20-25 C. (2-chloro-5-(trifluoromethyl)phenyl) methanol (compound of formula 13) (17.5 g, 84 mmol), and boronic acid 5 (Scheme 3 ) (18.1 g, 85 mmol) are added to the K2C03 followed by THF (100 mL) rinse. The solution is degassed by sparging with argon gas for 20 min. The catalyst, 1 ,1 bis(di-tert- butylphosphino)ferrocene palladium dichloride (300 mg, 0.55 mol%) is added. The organic layer tums dark brown immediately. The biphasic mixture is aged at 35-45 C with vigorous stirring for 32 hours. The mixture is cooled to room temperature and water (150 mL) is added, followed by petrol ether (150 mL) and the aqueous layer is removed. The organic layer was washed with water (2><200 mL) and filtered through silica gel and the solvent is removed under reduced pressure to yield brownish oil which is crystallized from heptane to give a pale white solid (28.5 g, 80%). mp 93.5-95.5 C; 1H NMR (CDCI3) delta 1.24 (d, J = 6.9 Hz, 6H), 1 .95 (t, J = 6.1 Hz, 1 H), 3.21 (sept, J = 6.9 Hz, 1 H), 3.73 (s, 3H), 4.49 (m, 2H), 6.68 (d, J = 12.0 Hz, 1 H), 6.99 (d, J = 8.6 Hz, 1 H), 7.30 (d, J = 7.9 Hz, 1 H), 7.59 (dd, J1 = 8.0 Hz, J2 = 1 .3 Hz, 1 H), 7.86 (d, J = 0.7 Hz, 1 H). The impurity (5'-ethyl-4'-fluoro-2'-methoxy-4-(trifluoromethyl)biphenyl-2-yl)methanol (~ 3 %), which is formed from 5-ethyl-4-fluoro-2-methoxyphenylboronic acid present in the starting material under the conditions described in Step 5, was detected in the product. These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,64372-62-9, its application will become more common. Reference:
Patent; LEK PHARMACEUTICALS D.D.; HUMLJAN, Jan; MARAS, Nenad; WO2013/91696; (2013); A1;,
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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. 647-42-7, name is 3,3,4,4,5,5,6,6,7,7,8,8,8-Tridecafluorooctan-1-ol, molecular formula is C8H5F13O, 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. Application In Synthesis of 3,3,4,4,5,5,6,6,7,7,8,8,8-Tridecafluorooctan-1-ol

(3) In a 4-liter reactor equipped with electromagnetic stirring, a rectification column, a thermometer, a constant pressure dropping funnel, a separator, a condenser, etc., 2500 g of an intermediate product obtained by (2) (6.05 mol of a fluorine-containing alcohol) is added. 20 g of p-toluenesulfonic acid and 13 g of hydroquinone. StirThe temperature was raised to 90 C, and 413 g (5.74 mol) of acrylic acid was added dropwise thereto for 2 hours.At the end of the reaction, no significant water droplets were produced after 5 hours of continuous reaction.The fluorine-containing olefin and the unreacted fluoroalcohol are distilled off.Refining 2133 g of perfluorohexylethyl acrylate, the purity is 99.02%,The yield was 88.8%.

With the rapid development of chemical substances, we look forward to future research findings about 647-42-7.

Reference:
Patent; Jinan Qifu New Materials Co., Ltd.; Shandong Chemical Institute; Li Haijing; Zhang Liting; (6 pag.)CN108911983; (2018); A;,
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Related Products of 101597-25-5, Adding some certain compound to certain chemical reactions, such as: 101597-25-5, name is 1,1-Bis(4-methoxyphenyl)prop-2-yn-1-ol,molecular formula is C17H16O3, 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 101597-25-5.

Analogously to a literature procedure32 TMSCl (0.30mL, 2.4mmol) was added to a solution of alkyne 11g27 (0.46g, 1.7mmol), DMAP (11mg, 0.090mmol) and TEA (0.38mL, 2.7mmol) in THF (3mL) at 25C. After stirring for 4h at 25C the mixture was quenched with 85 H2O, extracted with Et2O, dried with Na2SO4 and evaporated to dryness. The crude product was purified by flash chromatography with PE/EtOAc (97:3). Colorless oil (510mg, 88%). IR (Film): =3283, 3000, 2956, 2903, 2836, 1607, 1585, 1507, 1464, 1441, 1415, 1303, 1249, 1195, 1172, 1119, 1079, 1035, 1024, 1006, 936, 916, 883, 842, 806, 782, 756, 636cm-1. 1H NMR (500MHz, CD2Cl2) delta 0.11 (s, 9H), 2.93 (s, 1H), 3.77 (s, 6H), 6.79-6.84 (m, 4H), 7.41-7.46 (m, 4H) ppm. 13C NMR (126MHz, CD2Cl2) delta 1.75, 55.77, 75.35, 76.94, 87.31, 113.71, 127.71, 139.29, 159.44ppm. HRMS (EI): [M]+ calcd. for C20H24O3Si, 340.1495; found 340.1486.

According to the analysis of related databases, 101597-25-5, the application of this compound in the production field has become more and more popular.

Reference:
Article; Toth, Krisztian; Hoefner, Georg; Wanner, Klaus T.; Bioorganic and Medicinal Chemistry; vol. 26; 22; (2018); p. 5944 – 5961;,
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Synthetic Route of 83647-43-2, 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.83647-43-2, name is (3-Bromo-2-methylphenyl)methanol, molecular formula is C8H9BrO, molecular weight is 201.0605, as common compound, the synthetic route is as follows.

To a flask charged with (3-bromo-2-methylphenyl)methanol (6.0 g, 30 mmol) was added a IM TFA solution of Thallium Trifiuoroacetate (16.2 g, 29.8 mmol). The mixture was stirred at RT overnight. Analysis by TLC showed no starting material remaining. The solvent was removed under vacuum, and the residue was pumped under high vacuum for 30 min to ensure complete removal of TFA. To the residue was then added Palladium(II) Chloride (529 mg, 2.98 mmol), Lithium Chloride (2.53 g, 59.7 mmol), Magnesium Oxide (2.41 g, 59.7 mmol), and MeOH (150 mL). The reaction was flushed with CO twice, and kept under CO at room temperature. Analysis by LC showed a big product spot within 2 hours. To this solution was added ethyl acetate to precipitate the salts. The black solution was filtered through a celite pad, washed with EtOAc, adsorbed onto silica and purified by silica gel chromatography to afford 5-bromo-4- methyl-2-benzofuran-l (3H)-one. 1H-NMR (500 MHz, CDCl3) delta ppm 7.71 (d, J= 8.0 Hz, IH), 7.58 (d, J= 8.0 Hz, IH), 5.25 (s, 2H), 2.37 (s, 3H).

The chemical industry reduces the impact on the environment during synthesis 83647-43-2, I believe this compound will play a more active role in future production and life.

Reference:
Patent; MERCK SHARP &amp;; DOHME CORP.; PASTERNAK, Alexander; SHAHRIPOUR, Aurash; TANG, Haifeng; TEUMELSAN, Nardos, H.; YANG, Lihu; ZHU, Yuping; WALSH, Shawn, P.; WO2010/129379; (2010); A1;,
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Electric Literature of 86770-74-3 , The common heterocyclic compound, 86770-74-3, name is 2-(2-(2-(2-Aminoethoxy)ethoxy)ethoxy)ethanol, molecular formula is C8H19NO4, 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 1-7 and HATU (147 mg) in DMF (1 mL) was added dropwise DIEA (135 muL) and tetraethylene glycol monoamine (45 muL). After stirring at room temperature for 5 h, the reaction was quenched by 10% aqueous citric acid, and the reaction mixture was extracted with EtOAc. The organic phase was washed with 1N HCl, brine, and saturated NaHC03. After drying over MgSO4 and filtration, solvent was removed with a rotary evaporator, and the mixture was purified by silica gel chromatography (DCM: MeOH=30: 1) to afford 1-27 in 70% yield. Q-TOF LC/MS m/z 609.3797 [M+H]+ (calcd. 608.37 for C32H52N2O9 [M]+); 1HNMR (400 MHz, CDCl3) delta -0.45 (1H, m), 0.685 (1H, m), 0.825 (6H, m), 1.13 (9H, s), 1.27-1.64 (6H, m), 1.94 (1H, m), 2.05 (1H, m), 2.64 (2H, m), 3.38-3.91 (16H, m), 4.07 (1H, t, J=8 and 12 Hz ), 4.25 (1H, m), 4.99 (1H, m), 6.35-7.06 (4H, aromatic H); 13C NMR (100 MHz, CDC13) delta 21.45, 24.12, 25.92, 28.20, 30.00, 31.10, 38.40, 39.51, 40.65, 49.28, 50.18, 52.77, 61.65, 69.98, 70.22, 70.60, 70.90, 72.60, 73.92, 80.30, 120.40, 123.35, 129.95, 132.23, 132.46, 159.12, 171.62, 173.23, 174.34.

The synthetic route of 86770-74-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; YALE UNIVERSITY; THE UNITED STATES OF AMERICA as represented by THE DEPARTMENT OF VETERANS AFFAIRS; SADEGHI, Mehran; YE, Yunpeng; KIM, Hye-Yeong; HUANG, Henry (Yiyun); TOCZEK, Jakub; (85 pag.)WO2017/177144; (2017); A1;,
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Electric Literature of 24034-73-9 , The common heterocyclic compound, 24034-73-9, name is (2E,6E,10E)-3,7,11,15-Tetramethylhexadeca-2,6,10,14-tetraen-1-ol, molecular formula is C20H34O, 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.

[0294] The resulting 2E-conjugated ester 8 was reduced to the corresponding 2E-alcohol 9 by means of a lithium aluminum hydride (LAtI) treatment, which was then converted into the corresponding 2E,6ES 1 QE-geranylgeranyS bromide 10 by means of phosphorus tribromide (PBr3) treatment in ethyl ether (EE) or with Ph3P and CBr4 in acetonitriie (ACN) at 0C. Furthermore, the interaction of carbanion (derived from ethyl acetoacetate 5 and sodium ethoxide) with the bromide 10 at 0C afforded the desired 2E.6E, 10E-gerany{geranyl ketoester 11, a precursor needed for 5E.9E, 13E-geraByigeranyl acetone 1. The subsequent ester hydrolysis and decarboxylation of ketoester 11 using aq. 5N KOH at 80C yielded the requisite 5E.9E, 13E-geranyJgeranyl acetone 1. TLC Rf: 0.28 (5% Ethyl Acetate in Hexanes); LC Retention time: 16.68 min; MS (m e): 313 [M – 18 + H]+, 331 (MH]+, 353 [M – Kj,

The synthetic route of 24034-73-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; COYOTE PHARMACEUTICALS, INC.; SERIZAWA, Hiroaki; WO2014/107686; (2014); A1;,
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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. 4464-18-0, name is Benzene-1,3,5-triyltrimethanol. A new synthetic method of this compound is introduced below., name: Benzene-1,3,5-triyltrimethanol

1 ,3,5-Tris(hydroxymethyl)benzene 15 (927 mg, 5.12 mmol) was suspended in CH2CI2 (25 mL) and solid PCC (5.94g, 27.6 mmol) was added. After 30 minutes of stirring, the reaction was diluted with acetone (10 mL) and was allowed to stir for 3 hr at RT. TLC (10% MeOH, 90% CH2CI2 Rf=0.50) was used to determine if the reaction was complete. After the reaction was complete, the precipitated chromium salts were filtered off and washed with CH2CI2. The aqueous layer was extracted 3 times in CH2CI2 and saturated Na2CO3. The organic layers were combined and dried over anhydrous Na2SO4, filtered, and concentrated. Flash column chromatography (100% CH2CI2 Rf=0.4) gave 16 (272 mg, 1.68 mmol, 33%). 1H NMR (CDCI3): delta 10.21 (s, 3H), 8.63 (s, 3H).

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, 4464-18-0, Benzene-1,3,5-triyltrimethanol.

Reference:
Patent; UNIVERSITY OF CENTRAL FLORIDA RESEARCH FOUNDATION, INC.; PHANSTIEL, Otto; ARCHER, Jennifer, J.; WO2010/148390; (2010); A2;,
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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. 929-06-6, name is 2-(2-Aminoethoxy)ethanol, molecular formula is C4H11NO2, 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. HPLC of Formula: C4H11NO2

To a single-neck flask was added 2-(2-aminoethoxyl)ethanol (10.500 g). Tetrahydrofuran (25 mL) was added to dissolve 2-(2-aminoethoxyl)ethanol. Anhydrous sodium carbonate (5.300 g) was dissolved in distilled water (30 mL). The solution was added into the single-neck flask and cooled in an ice bath. Di-t-butyl dicarbonate (28.340 g) was dissolved in tetrahydrofuran (70 mL). The resultant solution was slowly dropwise added in the reaction system (for about 1 hr). After the addition, the mixture was stirred for 1.5 hr. After the reaction was completed, the reaction solution was filtered by suction. The filter cake was washed with tetrahydrofuran twice and then discarded. The filtrate was concentrated, then dissolved in ethyl acetate (150 mL) and distilled water (100 mL). The solution was mixed and then stood to separate. The aqueous phase was washed again with ethyl acetate (100 mL*2) twice. All the organic phases were combined, dried over MgSO4, filtered and concentrated to give the target compound.

With the rapid development of chemical substances, we look forward to future research findings about 929-06-6.

Reference:
Patent; Zhang, Hesheng; Huo, Aihong; Li, Zhenzhong; US2015/166595; (2015); A1;,
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Electric Literature of 928-51-8, 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. 928-51-8, name is 4-Chlorobutan-1-ol, molecular formula is C4H9ClO, 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: To a solution of DMSO (10ml) taken in a round bottom flask was added KOH (2equiv) and the solution was stirred at room temperature for 15min. The indole derivative 2 or 7 (1equiv) was then added and the mixture was further stirred for 1h, after which 4-chlorobutan-1-ol or 3-chloropropan-1-ol (1.5equiv) was added dropwise to the reaction mixture. The reaction was monitored by TLC to completion within 5h. The reaction mixture was then quenched by adding water and was extracted with ethyl acetate. Evaporation of the solvent under reduced pressure followed by column chromatography gave the required N-alkylated compounds, 3/8/12/16.

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 928-51-8, 4-Chlorobutan-1-ol.

Reference:
Article; Naik, Prajakta N.; Naik, Nilesh H.; Khan, Ayesha; Kusurkar, Radhika S.; Tetrahedron; vol. 69; 32; (2013); p. 6545 – 6551;,
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Related Products of 148043-73-6, 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. 148043-73-6, name is 4,4,5,5,5-Pentafluoropentan-1-ol, molecular formula is C5H7F5O, 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.

,4,5,5,5-pentafluoropentanol (10 g) and dichloromethane (100 mL) were added to the reaction flask, Triethylamine (11.3 g) was added and the mixture was added dropwise under ice-cooling Methylsulfonyl chloride (6.72 g) was added dropwise and the reaction was resumed at room temperature for 2 hours. Excess triethylamine and methylsulfonyl chloride were washed with water, dried over anhydrous sodium sulfate and spin dried to give 14.14 g 4,4,5,5,5-pentafluoropentanol methanesulfonate.

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 148043-73-6, 4,4,5,5,5-Pentafluoropentan-1-ol.

Reference:
Patent; Tianjin Pharmaceutical Innovation Co., Ltd.; LIU, WENJUAN; MO, LAN; (14 pag.)CN103965280; (2016); B;,
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