Month: July 2021

Electric Literature of 1454-85-9, 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.1454-85-9, name is Heptadecan-1-ol, molecular formula is C17H36O, molecular weight is 256.4672, as common compound, the synthetic route is as follows.

General procedure: The D1-OCn (n =15-21) were prepared as reported previously.22,23 The alkyl alcohol (1mmol) with triethylamine (2mmol) was added to isobutenyl binaphthyl di(acid chloride) (0.5mmol) in THF, and stirred at 60 °C for 1 day. After the evaporation of the solvent, the product was purified by silica gel column chromatography with CHCl3 as an eluent.

The chemical industry reduces the impact on the environment during synthesis 1454-85-9, I believe this compound will play a more active role in future production and life.

Reference:
Article; Kikkawa, Yoshihiro; Ishitsuka, Manami; Omori, Kazuhiro; Kashiwada, Ayumi; Tsuzuki, Seiji; Hiratani, Kazuhisa; Bulletin of the Chemical Society of Japan; vol. 88; 6; (2015); p. 834 – 842;,
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Reference of 109-83-1, 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 109-83-1, name is 2-(Methylamino)ethanol. This compound has unique chemical properties. The synthetic route is as follows.

To a solution of carbon disulfide (452 pL, 7.5 mmol, 1.5 eq.) in 10 mL anhydrous THF under intert atomsphere of argon, is added dropwise at 0 C 2-(methylamino)ethanol (400pL, 5.0 mmol, 1.0 eq.). After stirring atO Cfor5 minutes, sodium hydride (60% dispersion inmineral oil, 200 mg, 5.0 mmol, 1 .0 eq.) is added in portions. After 30 minutes of stirring at 0 0C the mixture is concentrated under reduced pressure and washed with cyclohexane toremove mineral oil and dried overnight under reduced pressure to yield a pale yellow powder (842 mg, 4.9 mmol, 97 % yield).1H NMR (400 MHz, MeOD) 6 (ppm): 3,57 (s, 3H, CH3), 3,87 (t, J = 6 Hz, 2H, CH2N),4,27 (t, J = 6 Hz, 2H, CH2O)130 NMR (100 MHz, MeOD) 6 (ppm): 44,7 (CH3N), 59,1 (CH2N), 61,2 (CH2O), 214,0 (CS2).

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 109-83-1, 2-(Methylamino)ethanol.

Reference:
Patent; UNIVERSITE PARIS EST CRETEIL VAL DE MARNE; CENTRE NATIONAL DE LA RECHERCHE SCIENTIFIQUE (CNRS); INSTITUT NATIONAL DE LA SANTE ET DE LA RECHERCHE MEDICALE (INSERM); MOTTERLINI, Roberto; FORESTI, Roberta; MARTENS, Thierry; RIVARD, Michael; WO2015/140337; (2015); A1;,
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Adding a certain compound to certain chemical reactions, such as: 927-74-2, 3-Butyn-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, 927-74-2, blongs to alcohols-buliding-blocks compound. Application In Synthesis of 3-Butyn-1-ol

To a stirred solution of the product of Preparation 19 (4.5 g, 16.3 mmol) in diethylamine (100 mL) was added but-3-yn-1-ol (1.9 mL, 32.6 mmol), Pd(PPh3)2Cl2 (500 mg, 1.63 mmol) and CuI (154 mg, 0.815 mmol) and resulting mixture was stirred for 17 h at room temperature. The solvent was then removed under reduced pressure and the residue was dissolved in diethyl ether (200 mL) and this solution was filtered to remove salts. The solvent was then removed under reduced pressure and the crude product was purified by silica gel chromatography (60% EtOAc/Hexane) to afford the title intermediate (3.03 g, 91% yield).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,927-74-2, its application will become more common.

Reference:
Patent; Mammen, Mathai; Mischki, Trevor; Hughes, Adam; Ji, Yu-Hua; US2006/35933; (2006); A1;,
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Reference of 929-06-6, Adding some certain compound to certain chemical reactions, such as: 929-06-6, name is 2-(2-Aminoethoxy)ethanol,molecular formula is C4H11NO2, 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 929-06-6.

Compound 35A: tert-butyl (2-(2-hydroxyethoxy)ethyl)carbamate O / (Boc)20 HzN^^^ ^”^^OH *~ BocHN’ THF 2-(2-aminoethoxy)ethanol (5 g, 47.56 mmol, 1.00 equiv) was dissolved in THF (100 mL) at 0C and sodium hydroxide (2 g, 50.00 mmol, 1.05 equiv) was then added (solution in 25 mL of water). A solution of di-tert-butyl dicarbonate (10.38 g, 47.56 mmol, 1.00 equiv) in THF (20 mL) was added drop-wise and the reaction was then left under agitation overnight at ambient temperature. The reaction was diluted by adding 50 mL of water and the product was extracted with 3 times 75 mL of AcOEt. The organic phases were combined, washed once with 100 mL of NaCl (sat.), then dried over sodium sulfate, filtered and concentrated under reduced pressure to yield 9 g (92 %) of compound 35A in the form of a yellow oil.

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. 929-06-6, 2-(2-Aminoethoxy)ethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; PIERRE FABRE MEDICAMENT; RILATT, Ian; PEREZ, Michel; GOETSCH, Liliane; BROUSSAS, Matthieu; BEAU-LARVOR, Charlotte; HAEUW, Jean-Francois; WO2015/162293; (2015); A1;,
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Reference of 624-95-3 , The common heterocyclic compound, 624-95-3, name is 3,3-Dimethylbutan-1-ol, 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.

[00066] Example V represents an oxidation in which the KBr co-catalyst and the NaHCO3 buffer were removed and they were replaced with Na2B4O7-Zr(acetate)2 additive. [00067] 16.9 g of 3,3-Dimethyl-1-butanol (117.3 mmol) and 0.0765 g MeO TEMPO (0.411 mmol) are charged in a jacketed glass reaction flask as in Example I. Sodium borate (0.380 g, 1.0 mmol) and Zr(acetate)2 (0.2 g solution, 0.1 mmol) are dissolved in water (12.0 cc) and the aqueous solution is added to the stirred organic fraction at 1000 RPM in the reaction flask. The stirred suspension is cooled to 0 C. and the emulsion is re-adjusted to pH=8.4 using 50% solution of CH3COOH. When the temperature of the reactants reached 0 C., 75.5 g (122 mmol) of 12.1% aqueous NaOCl solution are pumped in via a gas-tight syringe over 90 minutes (The pH of the bleach solution was adjusted to 10 using 50% aqueous CH3COOH). During the bleach addition the pH was maintained at 8.3-8.4 levels using few drops of 50% aqueous CH3COOH. The reaction mixture is stirred for an additional 120 min at 0 C. and the organic layer is sampled for GC assay. The reaction in this second stage was kept at pH 8.4 by addition of 0.2-0.25 cc aqueous solution of NaOH (50% concentration). The yield of 3,3-dimethylbutyraldehyde is 95.0% at 60 min and 93.0% at 90 min reaction time

The synthetic route of 624-95-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; The NutraSweet Company; US6825384; (2004); B1;,
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Application of 558-42-9, 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.558-42-9, name is 1-Chloro-2-methyl-2-propanol, molecular formula is C4H9ClO, molecular weight is 108.5667, as common compound, the synthetic route is as follows.

General procedure: In a150 mL pressure vessel, a suspension of 3-bromo-1H-pyrazole (8 g, 54.43 mmol) cesiumcarbonate (53.2 g, 163.29 mmol), and difluoroiodomethane (10percent wt. in THF, 200 ml, 106.23mmol) was heated at 45°C overnight. The reaction mixture was cooled to room temperature andthen filtered through Celite. The filter cake was washed with Et20 (3 x 150 mL). The filtrate was washed with brine, dried over sodium sulfate and carefully concentrated (20 °C bath, 100 mb vacuum) to give 17 g of a 1.5:1 ratio of regioisomers and solvent still present. This crude material was combined with 3,5-Difluoro-4-formylphenylboronic acid (12.65 g, 68.03 mmol),Palladium acetate (0.31 g, 1.381 mmol), butyldi- 1 -adamantylphosphine (1.171 g, 3.265 mmol) and Potassium carbonate (22.80 g, 164.96 mmol) in dioxane (150 mL) and water (50 mL) the mixture was degassed for 10 mm with argon, then heated at 100 °C overnight. The reaction mixture was cooled to room temperature, concentrated under reduce pressure, the residue was diluted with EtOAc and washed with brine 2x then dried over Na2504, filtered and concentratedunder reduced pressure. The crude residue was purified by silica column chromatography (5percent to15percent EtOAc/Hex). Mixed fractions were recrystallized (5:1 Hex/EtOAc) combined pure product afforded P4. 1HNMR (400 MHz, Chloroform-d) oe 10.35 (d, J = 1.0 Hz, 1H), 7.92 (d, J = 2.8 Hz, 1H), 7.46 (d, J = 9.6 Hz, 2H), 7.24 (t, J = 60.5 Hz, 1H), 6.80 (d, J = 2.8 Hz, 1H).

Statistics shows that 558-42-9 is playing an increasingly important role. we look forward to future research findings about 1-Chloro-2-methyl-2-propanol.

Reference:
Patent; GILEAD SCIENCES, INC.; BACON, Elizabeth M.; CHIN, Elbert; COTTELL, Jeromy J.; KATANA, Ashley Anne; KATO, Darryl; LINK, John O.; SHAPIRO, Nathan; TREJO MARTIN, Teresa Alejandra; YANG, Zheng-Yu; (395 pag.)WO2018/145021; (2018); 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. 517-21-5, name is Sodium 1,2-dihydroxyethane-1,2-disulfonate, molecular formula is C2H4Na2O8S2, 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. name: Sodium 1,2-dihydroxyethane-1,2-disulfonate

Glyoxal-sodium bisulfite (2.72 g, 10.2 mmol) was added to a solution of 3-amino-5-methyl-1H-pyrazole (2 g, 20.6 mmol) in water (40 mL) and was heated to 70 C. for 25 min. The mixture was then cooled down to room temperature and sodium cyanoborohydride (2.73 g, 43.4 mmol) was added and the mixture was stirred overnight. Methanol (70 mL) was added and the mixture was stirred for 1 h. Concentrated hydrochloric acid (12 N) was added until a pH<2 was obtained and the resulting mixture was stirred at room temperature overnight. The solution was then neutralized with an aqueous solution of sodium hydroxide (1M) and the solvent was evaporated. The residue was resuspended in methanol (40 mL) and stirred for 1 h. After filtration, the solvent was evaporated and the residue was purified by chromatography on a silica gel column (eluent: EtOAc, EtOAc-MeOH, 95:5, 90:10); N1,N2-bis(5-Methyl-1H-pyrazol-3-yl)ethane-1,2-diamine was obtained as a white solid.1H NMR (400 MHz, CDCl3): delta=2.21 (s, 6H), 3.35 (s, 4H), 5.35 (s, 2H).13C NMR (100 MHz, CDCl3/CD3OD 10:1): delta=11.29, 43.86, 89.75, 142.32, 155.13.MS (ESI): m/z=221 (MH+). With the rapid development of chemical substances, we look forward to future research findings about 517-21-5. Reference:
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Electric Literature of 504-63-2 ,Some common heterocyclic compound, 504-63-2, molecular formula is C3H8O2, 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.

Add hexadecane bromide (1.52 g, 5 mmol) to the reaction flask.And 1,3-propanediol (1.14 g, 15 mmol),Add 5 ml of dimethyl sulfoxide and 5 ml of tetrahydrofuran to dissolve.Add sodium hydroxide (800mg, 20mmol)The reaction was carried out for 24 hours at room temperature.Dilute with 10 ml of water,Adjust the pH to neutral with 2M dilute hydrochloric acid,Extracted with ethyl acetate 3 times,Combine the organic phase,Washed with saturated brine and concentrated.Purified by silica gel column chromatography to give compound 1.0g, Yield: 66.7%.

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. 504-63-2, 1,3-Propanediol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Shenzhen Tajirui Bio-pharmaceutical Co., Ltd.; Wang Yihan; Zhao Jiuyang; (46 pag.)CN109485676; (2019); A;,
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In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 2568-33-4, name is 3-Methylbutane-1,3-diol, the common compound, a new synthetic route is introduced below. category: alcohols-buliding-blocks

To a 50 mL three-necked flask equipped with a side tower packed column charged with 20 g of molecular sieve (4 A), a condenser, a thermometer and a drying tube, 0.26 g of the iron salen complex obtained in Production Example 1, 1.04 g of isoprene glycol (10 mmol),40 g (400 mmol) of methyl methacrylate and 0.08 g of phenothiazine were charged, the flask was immersed in an oil bath set at 120 C. under atmospheric stirring conditions so that the internal temperature of the flask was 100 to 105 C., The distillate fraction was fully refluxed through molecular sieves and transesterification reaction was carried out for 11 hours while returning to the reaction system. Composition analysis of the obtained reaction solution according to Test Example 1 revealed that isoprene glycol was not detected, isoprene glycol monomethacrylate was 0.1%, and isoprene glycol dimethacrylate was 99.9%. To this reaction solution, unreacted methyl methacrylate was distilled off using a rotary evaporator, 5 g of hexane was added, and the precipitated solid was suction filtered using filter paper (removal of solid matter). 5 g of 10 w / v% nitric acid aqueous solution was added to the obtained filtrate, and washing was carried out by mixing and the aqueous layer was removed by separation (washing with an acidic solution). Saturated sodium bicarbonate water was added to the obtained hexane solution to neutralize until the pH became 7. Hexane was distilled off from the hexane solution obtained by liquid separation to obtain 2.05 g of the objective isoprene glycol dimethacrylate.Composition analysis of the obtained target product according to Test Example 1 revealed that isoprene glycol was not detected, isoprene glycol monomethacrylate was 0.1%, and isoprene glycol dimethacrylate was 99.9%. The results evaluated according to Test Examples 1 to 3 are shown in Table 1.

The synthetic route of 2568-33-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; KURARAY COMPANY LIMITED; TAKAHATA, YUSUKE; KAJIYASHIKI, TSUYOSHI; HOSOKI, TOMOYA; (21 pag.)JP2018/104360; (2018); A;,
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Related Products of 4704-94-3 ,Some common heterocyclic compound, 4704-94-3, molecular formula is C4H10O3, 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 2-hydroxymethyl-1,3-propanediol (20 g,189 mmol) in dry acetone (600 ml) freshly annealed molecularsieves (4A) and p-toluenesulfonic acid monohydrate (2 g,10.5 mmol) were added. Reaction mixture was stirred overnightat room temperature. Mixture was filtered over kieselguhr. Tothe filtrate DOWEX (D1 OH-, 7 g) was added and the mixture washeated to 40 C and stirred for 30 min. Suspension was filtered overfrit (S3) and Et3N (0.5 ml) was added to the filtrate for stabilization.Solvent was evaporated in vacuo and obtained crude material wasdried under vacuum. Crude product 24 was obtained as colourlessoil and used in the next reaction step without purification. Reactionwas monitored by TLC.

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. 4704-94-3, 2-(Hydroxymethyl)propane-1,3-diol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; ?pa?ek, Petr; Keough, Dianne T.; Chavchich, Marina; Dra?insky, Martin; Janeba, Zlatko; Naesens, Lieve; Edstein, Michael D.; Guddat, Luke W.; Hockova, Dana; Bioorganic and Medicinal Chemistry; vol. 25; 15; (2017); p. 4008 – 4030;,
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