Author: tianli

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. 6149-41-3, name is Methyl 3-hydroxypropanoate. This compound has unique chemical properties. The synthetic route is as follows. Application In Synthesis of Methyl 3-hydroxypropanoate

Example 16 This example describes the preparation of various alkyl acrylate esters by dehydrating 3-HP esters using various catalysts. A catalyst was placed in a 3-neck flask that was equipped with a temperature probe (in contact with the catalyst). A distillation column and receiving flask were attached so that the vapors formed during the reaction could be collected, and the catalyst was heated to the desired temperature. A solution of a 3-hydroxypropionic acid ester in the corresponding alcohol was added drop-wise directly onto the catalyst using a syringe. The liquid that distilled over was collected and analyzed by gas chromatography. The results, and corresponding experimental conditions are shown in the following table. Ester Catalyst Temperature Concentration Solvent Yield of Yield of (C) of Ester in Acrylic Acrylic Solvent ester (GC) acid (GC) – (%) (%) (%) Ethyl NaH2P04-Silica 275-EtOH 49 26 Ethyl NaH2PO4-Silica 250 35 EtOH 53 Ethyl NaH2PO4-Silica 250 50 EtOH 14 21 Ethyl NaH2PO4-Silica 180 40 EtOH 30 – Ethyl Copper-H3PO4 220 20 EtOH 50 50 Methyl NaH2PO4-Silica 280-MeOH 78 Methyl CuS04-Silica 280-MeOH 37 9 Methyl Cs2CO3-Silica 220 45 MeOH 49 – Butyl NaH2PO4-Silica 280 50 BuOH 40 Similar dehydration reactions were performed using 3-HP as the starting material and a flask containing heated catalyst in place of the GC: (a) Aqueous 3-HP was dehydrated to acrylic acid over NaH2PO4-Silica gel catalyst at 180C. Based on GC and HPLC analysis, the yield of acrylic acid was 90- 96%. (b) Aqueous 3-HP was dehydrated to acrylic acid over H3PO4-Silica gel catalyst at 180C. Based on GC and HPLC analysis, the yield of acrylic acid was 85-90%. (c) Aqueous 3-HP was dehydrated to acrylic acid over CuS04-Silica gel catalyst at 180C. Based on GC and HPLC analysis, the yield of acrylic acid was 73%. (d) Aqueous 3-HP was dehydrated to acrylic acid over Zeolite H-ss powder and 85% H3PO4 as the catalyst at 180C. Based on GC and HPLC analysis, the yield of acrylic acid was 71%. (e) Aqueous 3-hydroxyisobutyric acid was dehydrated to methacrylic acid over NaH2PO4-Silica gel catalyst at 270C. Based on GC analysis, the yield of methacrylic acid was 79%.

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, 6149-41-3, Methyl 3-hydroxypropanoate.

Reference:
Patent; CARGILL, INCORPORATED; WO2003/82795; (2003); A2;,
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Synthetic Route of 30379-58-9, 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.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.

To a solution of anhydrous CH2Cl2 (3 mL), 4 A mol. sieves (0.1 g), protected glycolicacid 6 (150 g, 0.91 mmol) and compound 5 (500 g, 0.91 mmol) was added, at 20 C under argon atmosphere, TMSOTf (15 muL, 0,075 mmol). Afterwards the reaction mixture was stirred at this temperature for 3 h until TLC showed full conversion (PE:EtOAc 7:3, Rf 0.3). Than the mixture wasquenched by the addition of Et3N, filtered and the residue washed with CH2Cl2 (100 mL). The organic layer was concentrated. Pd-C catalyst was added to a solution of the oily mixture obtained from the previous reaction in 75 mL of (1:1) THF-MeOH. Afterwards, under stirring, the reaction mixture was placed under an H2 gas atmosphere (atmospheric pressure) and the deprotection of the benzyl ester was continued overnight. When full conversion had taken place (TLC examination), the H2 flow was replaced by Argon and the reaction mixture was filtered and washed (MeOH, 200 mL) through a pad of Celite. Upon concentration of the filtrate, a white solid material was obtained, and added CH2Cl2 was evaporated to remove traces of MeOH to afford 7 as a white solid (274 g, 0.6 mmol, 65% yield).

The chemical industry reduces the impact on the environment during synthesis 30379-58-9, I believe this compound will play a more active role in future production and life.

Reference:
Article; Ghidini, Alice; Steunenberg, Peter; Murtola, Merita; Stromberg, Roger; Molecules; vol. 19; 3; (2014); p. 3135 – 3148;,
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Related Products of 402-63-1, 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 402-63-1, name is 1-(3-Fluorophenyl)ethanol. This compound has unique chemical properties. The synthetic route is as follows.

General procedure: The catalyst solutionwas prepared by dissolving complex 3(36.1 mg,0.05mmol) in methanol (5.0 mL).Under a nitrogen atmosphere, the mixture of an alcohol substrate (2.0 mmol) and1.0 mL of the catalyst solution (0.01mmol) in 20mL acetone was stirred at 56 Cfor 10 minutes. tBuOK(22.4mg, 0.2 mmol)was then added to initiate the reaction.At the stated time, 0.1 mL of the reaction mixture was sampled and immediately diluted with 0.5 mL acetone pre-cooled-to-0 C for GC or NMR analysis. After the reaction was complete, the reaction mixture was condensed under reduced pressure and subject to purification by flash silica gel column chromatography to afford the corresponding ketone product, which was identified by comparison with the authentic sample through NMR and GC analysis.

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 402-63-1, 1-(3-Fluorophenyl)ethanol.

Reference:
Article; Wang, Qingfu; Du, Wangming; Liu, Tingting; Chai, Huining; Yu, Zhengkun; Tetrahedron Letters; vol. 55; 9; (2014); p. 1585 – 1588;,
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Related Products of 623-04-1, Adding some certain compound to certain chemical reactions, such as: 623-04-1, name is (4-Aminophenyl)methanol,molecular formula is C7H9NO, 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 623-04-1.

General procedure: To a solution of particular aromatic amine in 1,4-Dioxane (at the rate of 50 mg/ml) at -15.0 C, 5 equivalents of 2 M Sulphuric acid was added in small instalments while stirring. After 5 min 2 equivalents of 3 M sodium nitrite was added drop wise and after 30 min 3 equivalents of 3 M sodium azide was added drop wise carefully. Reaction was brought to room temperature and extracted with diethyl ether for at least three times. Organic layers were washed with saturated sodium bicarbonate solution two times, dried over anhydrous sodium sulphate and concentrated to a minimum volume under reduced pressure on Rotary evaporator without making use of heating from water bath.

According to the analysis of related databases, 623-04-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Farooq, Saleem; Shakeel-U-Rehman; Hussain, Aashiq; Hamid, Abid; Qurishi, Mushtaq A.; Koul, Surrinder; European Journal of Medicinal Chemistry; vol. 84; C; (2014); p. 545 – 554;,
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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.928-92-7, name is 4-Hexen-1-ol, molecular formula is C6H12O, molecular weight is 100.16, as common compound, the synthetic route is as follows.Formula: C6H12O

trans-4-hexene-1-ol(16, 40.0 g, 0.4 mol) and Et3N (48.5 g, 0.48 mol) weredissolved in toluene 400 mL. MsCl (50.3 g, 0.44 mol) was then dropped into this solution,which was cooled with ice, keeping the reaction temperature at 25C or less. After agitatingfor 1 hr, brine 200 mL was added. The organic layer was washed twice using 5 wt%NaHCO3 solution 500 mL and water 500 mL. After drying with MgSO4, the toluene wasconcentrated. As a result, 4-hexene-1-mesylate (17, 69.5 g, 0.39 mol, yield: 97.5%) wasobtained as a colorless, oily substance.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,928-92-7, 4-Hexen-1-ol, and friends who are interested can also refer to it.

Reference:
Article; Gotoh, Yasuyuki; Ushioda, Makoto; Molecular Crystals and Liquid Crystals; vol. 593; 1; (2014); p. 61 – 77;,
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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 162358-05-6, name is 2-(4-Octylphenyl)ethanol. This compound has unique chemical properties. The synthetic route is as follows. name: 2-(4-Octylphenyl)ethanol

Example 17 Preparation of 4-octylphenethyl methanesulfonate 2-(4-Octylphenyl)ethanol (53 g) and dichloromethane (500 mL) are charged into a 1 liter three-neck round bottom flask equipped with guard tube and addition funnel. Triethylamine (83.5 g) is added, the mixture is stirred for 30 minutes, then it is cooled to 0 C. Methanesulphonyl chloride (35.2 mL) is added drop-wise at 0 C. and the mass is stirred for 3 hours at room temperature. The mass is diluted with water (700 mL) and the organic layer is separated and the aqueous layer is extracted with dichloromethane (2*250 mL). The combined organic layers is washed with saturated sodium bicarbonate (500 mL) and brine solution (500 mL). The organic layer is separated, dried with sodium sulphate, and concentrated under vacuum to obtain the title compound. Yield: 70 g.

With the rapid development of chemical substances, we look forward to future research findings about 162358-05-6.

Reference:
Patent; DR. REDDY’S LABORATORIES LTD.; Katkam, Srinivas; Sagyam, Rajeswar Reddy; Morthala, Raghavendar Rao; Ireni, Babu; Vinigari, Krishna; Ramdoss, Suresh Kumar; Rangineni, Srinivasulu; Tummala, Arjunkumar; Iqbal, Javed; Oruganti, Srinivas; Kandagatla, Bhaskar; US2014/235895; (2014); A1;,
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Electric Literature of 261762-59-8 ,Some common heterocyclic compound, 261762-59-8, molecular formula is C7H6ClFO, 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 the compound of Reference Example 1 (100 mg, 0.32 mmol) in 1,4-dioxane (0.64 mL) was added (2-chloro-5-fluorophenyl) methanol (120 mg, 0.74 mmol), sodium hydride , 0.80 mmol) at room temperature, and the mixture was stirred at 100 C. for 48 hours. Water (10 mL) was added to the reaction mixture at room temperature and extracted with ethyl acetate (10 mL × 2). The organic layers were combined, dried over sodium sulfate and concentrated. The resulting concentrate was purified by silica gel column chromatography (eluent: ethyl acetate / n-hexane = 30/70) to give an intermediate as a yellow oil (80 mg).To a solution of the obtained intermediate (80 mg) in 1,4-dioxane (0.32 mL) was added 4 N hydrogen chloride 1,4-dioxane solution (0.8 mL) at room temperature, and the mixture was stirred at room temperature for 1 hour. Acetonitrile (5.0 mL) was added to the reaction mixture at room temperature, diethyl ether (1.5 mL) was added dropwise at room temperature, and the mixture was stirred at room temperature for 1 hour. The solid was collected by filtration and dried under reduced pressure at room temperature to give 1- (6 – ((2-chloro-5-fluorobenzyl) oxy) pyrazin-2-yl) -1, 4- diazepane dihydrochloride Compound of Example 8) as a white solid (40 mg, 31% yield).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 261762-59-8, 2-Chloro-5-fluorobenzyl alcohol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; TORAY INDUSTRIES INCORPORATED; KIKUCHI, TSUKASA; OKANO, TSUBASA; (24 pag.)JP2017/14121; (2017); A;,
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Electric Literature of 19812-64-7, 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. 19812-64-7, name is Tetradecane-1,14-diol. A new synthetic method of this compound is introduced below.

Synthesis Example D-(25) 1,14-Tetradecandiol (1.5 g) was dissolved in 16.5 ml of cyclohexane, and 57% aqueous hydrobromic acid solution (16.5 ml) was added to this solution. The reaction mixture was refluxed for six hours while stirring. After the reaction, the mixture was extracted three times with diethyl ether. The organic layer was neutralized with saturated sodium hydrogen carbonate solution, washed with saline solution, dried over magnesium sulfate, and filtered, and the solvent was distilled off under reduced pressure. Purification of the residue by silica gel flash chromatography (hexane: ethyl acetate = 7:3) gave 14-bromotetradecan-1-ol as white crystals at a 67% yield. Molecular weight: 292.90 (C14H29BrO) TLC: (hexane-ethyl acetate 7-3) Rf value=0.53 1H-NMR: (300MHz, CDCl3) delta: 1.26 (s large, 20H, -(CH2)10-); 1.56 (qt, 2H, J=7.0Hz, -CH2-); 1.85 (qt, 2H, J=7.1Hz, -CH2-); 3.40 (t, 2H, J=6.9Hz, -CH2-Br); 3.64 (t, 2H, J=6.6Hz, -CH2-O-) 13C-NMR: (75MHz, CDCl3)delta: 25.72; 28.17; 28.75; 29.41-32.80; 32.82; 34.05; 63.08

At the same time, in my other blogs, there are other synthetic methods of this type of compound,19812-64-7, Tetradecane-1,14-diol, and friends who are interested can also refer to it.

Reference:
Patent; Meiji Dairies Corporation; EP1854777; (2007); A1;,
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Application of 2979-22-8 ,Some common heterocyclic compound, 2979-22-8, molecular formula is C9H12O2, 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: To a solution of the appropriate alcohol (10mmol) in dry CH2Cl2 (20ml) was added Bu2SnO (0.2mmol) followed by the addition of pTsCl e (10mmol) and TEA (10mmol). The reaction mixture was kept under vigorous stirring at rt for 1-6h. The reaction mixture was quenched by adding water. The solution was extracted with dichloromethane and then combined organic phase were washed with a saturated aqueous solution of brine and dried over anhydrous Na2SO4. The solvent removing in vacuo give a residue that was crystallized or chromatographed to afford the desired compounds (1-5).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,2979-22-8, its application will become more common.

Reference:
Article in Press; Pasquinucci, Lorella; Turnaturi, Rita; Prezzavento, Orazio; Arena, Emanuela; Arico, Giuseppina; Georgoussi, Zafiroula; Parenti, Rosalba; Cantarella, Giuseppina; Parenti, Carmela; Bioorganic and Medicinal Chemistry; (2017);,
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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. 16545-68-9, name is Cyclopropanol. A new synthetic method of this compound is introduced below., Safety of Cyclopropanol

To a solution of 1.5 g (7.44 mmol, 1.0 eq.) of 4-nitrophenyl chloroformate in 25 mL ofmethylene chloride at 0C was added 0.5 g (8.61 mmol, 1.16 eq.) of cyclopropanol followedby 0.63 g (8.05 mmol, 1.08 eq) of pyridine. The resulting solution was stirred at 0 C for 1.5 h. The mixture was diluted with 5 mL of methylene chloride and 10 mL of 0.1 M aqueous sulfuric acid. The organic phase was then washed with 10 mL of sat. NaHCO3, 10 mL of water and 10 mL of brine. The organic phase was dried (Na2SO4), filtered and concentratedto a volume of approximately 5 mL, and 10 mL of cyclohexane was added. The resulting yellow solid was removed, and the filtrate was evaporated to provide 0.8 g (3.58 mmol, 48%) of cyclopropyl (4-nitrophenyl) carbonate. ?H NMR (400 MHz, CDC13): 8.26-8.19 (m, 2H), 7.34-7.25 (m, 2H), 4.25-4.19 (m, 1H), 0.85-0.69 (m, 4H).

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, 16545-68-9, Cyclopropanol.

Reference:
Patent; ARBUTUS BIOPHARMA CORPORATION; COLE, Andrew, G.; DORSEY, Bruce, D.; KAKARLA, Ramesh; KULTGEN, Steven; QUINTERO, Jorge; (353 pag.)WO2018/172852; (2018); A1;,
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