Author: tianli

Adding a certain compound to certain chemical reactions, such as: 2277-23-8, 2,3-Dihydroxypropyl decanoate, 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 2,3-Dihydroxypropyl decanoate, blongs to alcohols-buliding-blocks compound. Quality Control of 2,3-Dihydroxypropyl decanoate

Compound 1, 100 mg, compound 2, 76 mg,120 mg of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride (EDCI)42 mg of 1-hydroxybenzotriazole (HOBt) was dissolved in 2 ml of THF,The reactants were mixed and replaced with nitrogen three times,After stirring at room temperature for 1 hour.TLC detection (DCM: MeOH = 5: 1), the remaining starting material,The system was concentrated directly and scraped into large plates (DCM: MeOH = 10: 1) to give 51 mg of a light yellow oil.

The synthetic route of 2277-23-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Si Fenke Si Pharmaceutical Research And Development (Tianjin) Co., Ltd.; Yao Qingjia; Wu Simin; Xu Yangjun; (6 pag.)CN106749210; (2017); A;,
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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. 53463-68-6, name is 10-Bromodecanol, molecular formula is C10H21BrO, 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: C10H21BrO

To 2.00 g of 10-bromo-1-decanol in 15 mL of chloroform (CHCl3) was added dropwise 16.9 mmol of 3,4-dihydro-2H-pyran (DHP) and catalytic amounts of p-toluenesulphonic acid (pTSA). The reaction mixture was stirred for 24 h at room temperature. The organic layer was washed with water (2 .x. 20 mL), NaHCO3 (2 .x. 20 mL), CHCl3 (1 .x. 20 mL), and dried over MgSO4, filtered, and evaporated in vacuo. The crude product was purified using silica gel column chromatography eluting with hexane/ether (9:1). The pure product 2 (Banaszak et al., 2009) was obtained as a colorless oil 2.35 g (7.32 mmol) for a 100percent yield.

With the rapid development of chemical substances, we look forward to future research findings about 53463-68-6.

Reference:
Article; Carballeira, Ne?stor M.; Montano, Nashbly; Cintro?n, Gabriel A.; Ma?rquez, Carmary; Rubio, Celia Ferna?ndez; Prada, Christopher Ferna?ndez; Balan?a-Fouce, Rafael; Chemistry and Physics of Lipids; vol. 164; 2; (2011); p. 113 – 117;,
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Reference of 1454-85-9 , The common heterocyclic compound, 1454-85-9, name is Heptadecan-1-ol, molecular formula is C17H36O, 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.

In a 100 ml, 3 port reaction vessel equipped with a mechanical stirrer, mantle, thermowatch, short-column condenser, cow receiver, thermometers, and a nitrogen blanket, 27.68 grams of hydrophobe group containing compound and 4.34 grams of p-toluenesulfonic acid monohydrate were added. The reactants were heated to about 80° C. and 25 grams of the trithiocarbonate compound was added. A partial vacuum to 60 mmHg mercury was applied and the temperature was increased to about 110° C. for a period of five hours to produce the product shown above.

The synthetic route of 1454-85-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Lai, John Ta-Yuan; Hsu, Shui-Jen Raymond; Tamareselvy, Krishnan; US2006/39939; (2006); A1;,
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Related Products of 96-35-5 ,Some common heterocyclic compound, 96-35-5, molecular formula is C3H6O3, 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.

Example 1Reduction of Methyl Glycolate in Methanol to Ethylene Glycol The following example shows the positive effect of adding a promoter to the catalyst mixture. Run 1 in the table below is a comparative example. Runs 2-9 represent variants of the current invention.A 300-milliliter autoclave was charged with Ru(Acac)3 (0.10 mmole), TRIPHOS (0.50 mmole), and the promoter in the amount specified in the table. Methanol (32 milliliters) and methyl glycolate (0.156 mole) were added, and the reactor was sealed under N2. The reactor was pressurized to 250 psig (1.7 MPa) with H2 and heated to 200 C. Upon reaching 200 C., the H2 pressure was raised to 2000 psig (13.8 MPa). The autoclave was stirred and held at 200 C., 2000 psig (13.8 MPa) for a total of 3 hours. The autoclave was then cooled, excess gas vented, and the contents recovered. The contents were analyzed by the use of an internal standard gas chromatography method for the presence of methyl glycolate (?MG?) and ethylene glycol (?EG?). The results are shown in the table below. Catalyst Activity Rate Amount of Conversion of Selectivity to (moles EG per Promoter MG EG mole of Ru Run Promoter (mmole) (%) (%) per hr) 1 none none 39.5 88.4 205 2 Zn 0.25 49.3 88.9 228 Acetonylacetonate 3Me4NBF4 0.025 99.7 98.2 509 4Me4NBF4 0.001 96.8 98.2 394 5NH4PF6 0.025 100 96.9 504 6NH4OAc 0.150 67.8 94.8 334 7Ph4PBr 0.025 84.1 97.8 428 8NaPh4B 0.500 81.1 93.5 394 9BuN4PF6 0.025 97.8 95.8 487 Analysis of the run without a promoter showed a 39.5% conversion of the methyl glycolate with 88.4% selectivity to ethylene glycol. The catalyst activity rate for this experiment was 205 moles of EG per mole of ruthenium per hour. On the other hand, runs with a promoter showed MG conversions of 49-100%, EG selectivities of 89-98%, and catalyst activity rates of 230-510 moles of EG per mole of ruthenium per hour. This data show the positive effects of adding a promoter to the reaction mixture.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,96-35-5, its application will become more common.

Reference:
Patent; EASTMAN CHEMICAL COMPANY; US2009/143612; (2009); A1;,
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Related Products of 150192-39-5, 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. 150192-39-5, name is (2-Bromo-5-methoxyphenyl)methanol, molecular formula is C8H9BrO2, 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.

Example 2; 2- [(2-Bromo-5-methoxybenzyl) oxy]-7-methoxynaphthalene [0045]; To a solution of 7-methoxy-2-naphthol (26.92 g, 0.15 moles), 2-bromo- 5-methoxybenzyl alcohol (33.58 g, 0.15 moles), and triphenylphosphine (39.3 g, 0.15 moles) in anhydrous THF (500 mls) was added a solution of DEAD (26.10 g, 0.15 moles) in THE (100 mL) dropwise over 0.5 hr. The solution was stirred at room temperature overnight and, upon evaporation of half the volume, the product precipitated in good purity. The solid was filtered and rinsed with THF, then dried to yield 32.96 g (59%) of a white solid: mp 156-157 C ; 1H NMR (DMSO-d6): 6 3.77 (3H, s), 3.86 (3H, s), 5.18 (2H, s), 6.92 (1H, dd, J=3. 2 Hz, J=8. 7 Hz), 7.00 (1H, dd, J=2. 4 Hz, J=8. 7 Hz), 7.09 (1H, dd, J=2. 4 Hz, J=8. 9 Hz), 7.22 (1H, d, J=3. 2 Hz), 7.25 (1H, d, J=2. 4 Hz), 7.35 (1H, d, J=2. 4 Hz), 7.59 (1H, d, J=8. 7 Hz), 7.74 (1H, d, J=8. 7 Hz), 7.76 (1H, d, J=8. 7 Hz); MS mlz 373/375 ( [M+H] +). Anal. for ClsHl7BrO3 : Calc’d: C: 61.14 ; H: 4.59 Found: C: 61.29 ; H: 4.21

According to the analysis of related databases, 150192-39-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; WYETH; WO2005/82880; (2005); A1;,
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Synthetic Route of 16308-92-2, 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.16308-92-2, name is (2,4-Dimethylphenyl)methanol, molecular formula is C9H12O, molecular weight is 136.19, as common compound, the synthetic route is as follows.

General procedure: General procedure for the one-pot tandem oxidation-Wittig reaction To a flask containing BaMnO4 (1.2 mmol, 300 mg)and the alcohol (1 mmol) in CH3CN (5 mL) were added PPh3(1.2 mmol, 315 mg) and ethyl bromoacetate (1.2 mmol, 0.13 mL) and the mixturewas stirred at 80 C for 24 h. Then the obtained mixture was filtered and theresulting solution was subjected to column chromatography using n-hexane/ethylacetate to isolate the pure products in 78-93% isolated yields with highstereoselectivity.

Statistics shows that 16308-92-2 is playing an increasingly important role. we look forward to future research findings about (2,4-Dimethylphenyl)methanol.

Reference:
Article; Gholinejad, Mohammad; Firouzabadi, Habib; Bahrami, Maedeh; Najera, Carmen; Tetrahedron Letters; vol. 57; 33; (2016); p. 3773 – 3775;,
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Electric Literature of 1562-00-1, 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. 1562-00-1, name is Sodium isethionate. A new synthetic method of this compound is introduced below.

An electrically-heated, mechanically stirred 1 liter autoclave was fitted with an vent valve connected in turn to a condenser and receiver assembly, a bottom valve, a thermowell, a pressure gauge, an inlet line for feeding of reagents, and a pressure-relief valve. The receiver was placed on a balance to facilitate continuous determination of the amount of distillate collected in the receiver. The amine starting material, aqueous sodium 2-hydroxyethanesulfonate, and aqueous 50 percent sodium hydroxide were charged to the autoclave. With the isolation valve open, the reaction mixture was rapidly heated with stirring until condensate was detected in the condenser/receiver. The mixture was further heated with continuous removal of water until the targeted amount of distillate had been removed. An analysis of the collected aqueous distillate was performed by UV spectroscopy to determine the amount of amine which co-distilled with the water. The isolation valve was then closed and the reaction mixture further heated to a target temperature in the range of 140-200 C. for 2-17 hours as specified in Examples 1-8. The reaction mixture was then cooled until the pressure dropped to 0 psig (ca. 110 C.) whereupon dilution water was added to dilute the concentrated reaction product. The resulting solution was then cooled to room temperature and drained from the reactor. Analysis of the product mixture was then performed by various chromatographic and spectroscopic procedures as indicated in the specific examples.; Procedure C A magnetically-stirred 70-mL fluoropolymer-lined steel autoclave was fitted with an internal thermocouple capable of determining the temperature of the liquid phase contained in the vessel, a pressure gauge, a pressure-relief valve, and a vent valve. The amine starting material, anhydrous or aqueous sodium 2-hydroxyethanesulfonate, and anhydrous or aqueous sodium hydroxide were charged to the open autoclave, which was then assembled and immersed in an electrically heated oil bath. With the vent valve closed, the stirred reaction mixture was rapidly heated to the reaction temperature and held at that temperature for the times specified in Examples 9, 10, and 13 below. The reaction mixture was then cooled to ambient temperature, the reactor opened, and the reaction product taken up in sufficient water to dissolve all solids.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,1562-00-1, its application will become more common.

Reference:
Patent; Carroll, Glenn T.; Smith, Gary S.; Stringer, Gary E.; US2006/89509; (2006); A1;,
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Electric Literature of 1883-32-5, 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.1883-32-5, name is 2,2-Diphenylethanol, molecular formula is C14H14O, molecular weight is 198.26, as common compound, the synthetic route is as follows.

General procedure: A mixture of 3,4,6-tri-O-acetyl-D-glucal 1 (50.0 mg, 0.184 mmol) and alcohol (0.193 mmol) was dissolved in dry-CH2Cl2 : dry-toluene (125 : 200 muL) under gas-nitrogen. The solution was cooled to 0 C, then 0.5 M IBr in CH2Cl2 (20 mol%, 75 L) was added slowly. The stirring was continued at 0-20 C for 1-10 h. After TLC showed the completed conversion, the reaction mixture was quenched carefully with cooled aq.Na2S2O3 (20 mL) and washed with satd aq. NaHCO3 (20 mL), and extracted with EtOAc (3×20 mL). The combined organic layer was washed with brine (20 mL), dried over anhydrous Na2SO4, and then concentrated under reduced pressure. The residues were purified by silica gel column chromatography (EtOAc/n-hexane) to give the 2,3-unsaturated-O-glycoside products 2a-2t in good to high yields (71-99%). In most cases, a mixture of alpha and beta-anomers of glycoside 2 was obtained. The ratio of the isomers was determined by comparison of the integration values of the peaks in 1H NMR analysis. The alpha-configuration was characterized from the position of anomeric proton which appears in an up fieldposition compared to -anomer in most cases. The beta-isomers was not separated but characterized compared with the literature data of the mixture. Spectral data of pure alpha-isomers are as followed.

Statistics shows that 1883-32-5 is playing an increasingly important role. we look forward to future research findings about 2,2-Diphenylethanol.

Reference:
Article; Saeeng, Rungnapha; Siripru, Onanong; Sirion, Uthaiwan; Heterocycles; vol. 91; 4; (2015); p. 849 – 861;,
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Synthetic Route of 148043-73-6 , The common heterocyclic compound, 148043-73-6, name is 4,4,5,5,5-Pentafluoropentan-1-ol, molecular formula is C5H7F5O, 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.

Step-6.1: Synthesis of 4,4,5,5,5-pentafluoropentyl methanesulfonate To a stirred solution of 4,4,5,5,5-pentafluoropentan-l-ol (7.5 g, 42.13 mmol) in dichloromethane (100 mL) at 0 C was added triethylamine (7.1 mL, 50.56 mmol) and methane sulfonyl chloride (3.53 mL, 46.34 mmol). The reaction mixture was stirred for 1 h at RT and diluted with dichloromethane. The organic layer was washed with water, brine, dried over anhydrous Na2S04 and concentrated under reduced pressure to afford 4,4,5,5,5- pentafluoropentyl methanesulfonate (6.0 g, 56%) as a brown colour liquid.

The synthetic route of 148043-73-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; EISAI R&D MANAGEMENT CO., LTD.; HAO, Ming-Hong; KORPAL, Manav; NYAVANANDI, Vijay Kumar; PUYANG, Xiaoling; SAMAJDAR, Susanta; SMITH, Peter Gerard; WANG, John; ZHENG, Guo Zhu; ZHU, Ping; (161 pag.)WO2016/196342; (2016); A1;,
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Application of 94022-96-5 ,Some common heterocyclic compound, 94022-96-5, molecular formula is C9H9F3O, 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 mixture of alcohol 1 (1 mmol), the O, Se acetal 2a (1.4 mmol), solid potassium carbonate (2.0 mmol) and activated 3 A molecular sieves (0.20 g) in dry ethyl acetate (16 mL), solid N-iodosuccinimide (1.4 mmol) was added in portion at room temperature. The mixture was stirred under inert atmosphere and monitored by TLC. Reaction times ranged from 0.5 to 2 h. The brown colored reaction mixture was quenched into 20 mL of 10% aqueous sodium thiosulfate pentahydrate solution, mixed, and separated. The aqueous phase was extracted with 10 mL of ethyl acetate and the combined organic phases were washed with 10 mL of brine, dried over sodium sulfate and concentrated. Purification by silica gel column chromatography afforded the MOM-ether derivative 3.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,94022-96-5, its application will become more common.

Reference:
Article; Temperini, Andrea; Annesi, Diego; Testaferri, Lorenzo; Tiecco, Marcello; Tetrahedron Letters; vol. 52; 25; (2011); p. 3179 – 3182;,
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