Tag: M.W=0-100

Related Products of 2516-33-8 ,Some common heterocyclic compound, 2516-33-8, molecular formula is C4H8O, 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: The gas-phase selective oxidation of alcohols on these catalysts with molecular oxygen was carried out on a fixed-bed quartz tube reactor (i.d., 16 mm) under atmospheric pressure as described previously [14,15,26,27]. Circular chips (16.1 mm diameter) of the microfibrous-structured Au/Ni-fiber catalysts were punched down from their large sheet sample and packed layer-up-layer into the tube reactor with total mass of 0.3 g. Note that the diameter of 0.1 mm larger than the i.d. of the tubular reactor was retained deliberately to avoid the appearance of the gap between the reactor wall and the edges of the catalyst chips thereby preventing the gas bypassing. Alcohols were fed continuously using a high-performance liquid pump, in parallel with O2 (oxidant) and N2 (diluted gas) feeding using the calibrated mass flow controllers, into the reactor heated to the desired reaction temperature. The organic phase of the liquid effluent was collected for analyzing by an HP 5890 gas chromatography-flame ionization detector (GC-FID) with a 60-m HP-5 ms capillary column. The gas-phase products such as H2, COx, and C1-C3 hydrocarbons were analyzed by an HP-5890 GC with thermal conductivity detector (TCD) and a 30-m AT-plot 300 capillary column. Reaction temperature, WHSV, and alcoholic hydroxyl (O2/ol) were varied in range from 220 to 380 C, 10 to 70 h-1, and 0.4 to 1.2, respectively. Prior to the reaction testing, as-prepared catalysts were all activated by performing the benzyl alcohol oxidation at a high temperature of 380 C for 1 h, using molar ratio of O2 to O2/ol = 0.6 and WHSV = 20 h-1.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,2516-33-8, its application will become more common.

Reference:
Article; Zhao, Guofeng; Deng, Miaomiao; Jiang, Yifeng; Hu, Huanyun; Huang, Jun; Lu, Yong; Journal of Catalysis; vol. 301; (2013); p. 46 – 53;,
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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.3279-95-6, name is 2-(Aminooxy)ethanol, molecular formula is C2H7NO2, molecular weight is 77.08, as common compound, the synthetic route is as follows.Formula: C2H7NO2

Step C Preparation of 2-(2-chloro-4-iodo-phenylamino)-3,4-difluoro-N-(2-hydroxy-ethoxy)-benzamide To a solution of the product of Example 6, Step B, 2-(2-chloro-4-iodophenylamino)-3,4-difluorobenzoic acid pentafluorophenyl ester (10.0 g, 17.4 mmol), in anhydrous dimethylformamide (36 mL) was added 2-(aminooxy)-ethanol [prepared by the literature procedure: Dhanak, D.; Reese, C. B. J. Chem. Soc., Perkin Trans. 1 1987, 2829] (1.6 g, 20.8 mmol) and N,N-diisopropylethylamine (6.0 mL, 34.8 mmol). The resultant solution was stirred at ambient temperature for 16 h. The reaction mixture was concentrated to 20% volume then diluted with ethyl acetate (360 mL). The resultant solution was washed with water (6*60 mL) and brine (2*60 mL). The organics were dried over anhydrous magnesium sulfate and concentrated under reduced pressure to afford a white solid that was purified on silica gel. Elution with ethyl acetate-methanol (9:1) afforded 2-(2-chloro-4-iodo-phenylamino)-3,4-difluoro-N-(2-hydroxy-ethoxy)-benzamide (7.31 g, 90%) as a white solid. Recrystallization from methanol afforded analytically pure material: m.p. 173-175 C.; 1H NMR (400 MHz, DMSO-d6) delta 11.93 (br s, 1H), 8.85 (br s, 1H), 7.76 (d, J=1.7 Hz, 1H), 7.48 (dd, J=8.6, 1.7 Hz, 1H), 7.44 (dd, J=8.5, 6.2 Hz, 1H), 7.25 (dt, J=8.5, 9.3 Hz, 1H), 6.58 (dd, J=8.5, 6.4 Hz, 1H), 4.70 (br s, 1H), 3.86 (br s, 2H), 3.56 (br d, J=3.9 Hz, 2H); MS (APCI+)=469.0; MS (APCI-)=467.0; Anal. Calcd/found for C15H12ClF21N2O3: C, 38.45/38.60; H, 2.58/2.53; N, 5.98/5.91; F, 8.11/8.08; I, 27.08/27.43. aa0-5aa

At the same time, in my other blogs, there are other synthetic methods of this type of compound,3279-95-6, 2-(Aminooxy)ethanol, and friends who are interested can also refer to it.

Reference:
Patent; Barrett, Stephen Douglas; Kaufman, Michael David; Rewcastle, Gordon William; Spicer, Julie Ann; US2003/232889; (2003); 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. 3513-81-3, name is 2-Methylenepropane-1,3-diol. A new synthetic method of this compound is introduced below., Formula: C4H8O2

Preparation 3 3-Octadecylaminocarbonyloxy-2-methylenepropan-1-ol Octadecyl isocyanate (59.1 g) and 2-methylene-propane-1,3-diol (17.7 g) were dissolved and stirred in pyridine (100 ml) for 24 hours at 22°C. Water (200 ml) was added, and the mixture was extracted with chloroform (3 * 200 ml). The chloroform extracts were washed with water, dried over anhydrous magnesium sulfate, filtered and evaporated to dryness in vacuo . The mixture was purified through a column of silica gel 60 (70-230 mesh, 100 g) eluding with chloroform/ether 1: 1. Further purification was achieved by chromatography on a Waters PrepLC.(R)./System 500A using a PrepPAK.(R).-500/SILICA cartridge with chloroform/ether/pentane 1: 1: 3 as eluent. The product was recrystallized from acetone. Mp. 71-73°C. Elemental analysis: calculated C 71.99percent, H 11.82percent, N 3.65percent, found C 71.93percent, H 11.93percent, N 3.64percent.

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, 3513-81-3, 2-Methylenepropane-1,3-diol.

Reference:
Patent; LEO PHARMACEUTICAL PRODUCTS LTD. A/S, (LOVENS KEMISKE FABRIK PRODUKTIONSAKTIESELSKAB); EP247201; (1991); B1;,
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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, category: alcohols-buliding-blocks, blongs to alcohols-buliding-blocks compound. category: alcohols-buliding-blocks

(But-3-yn- 1 -yloxy) (tert-butyl)dimethylsilane (3.5) [00139] Compound 3.5 was synthesised using a similar procedure by Nadeau et al. To a solution of 3-butyn-1 -ol (3.00 g, 42.8 mmol) in dichloromethane (60 mL) was added imidazole (7.28 g, 107 mmol) and cooled to 5 C. tert-Butyldimethylsilyl chloride (6.45 g, 42.8 mmol) was added and the reaction mixture was stirred at 25 C for 1 6 hours. Dichloromethane (100 mL) was added and the mixture was washed with water (2 x 50 mL) and brine (50 mL). The organic layer was dried over magnesium sulfate, filtered and concentrated in vacuo to afford compound 3.5 (7.73 g, 98%) as a colourless oil. 3.5: C10H20OSi (Mr 184.35); 1H NMR (400 MHz, CDCI3) O (ppm) 3.74 (t, J=7.1 Hz, 2H), 2.40 (td, J= 7.1, 2.7 Hz, 2H), 1 .95 (t, J= 2.7 Hz, 1 H), 0.90 (5, 9H),0.07 (5, 6H); 13C NMR (101 MHz, CDCI3) O (ppm) 81.6, 69.4, 61.9, 26.0, 23.0,18.4, -5.2. Does not ionise in ESI-MS. Nb. 1H NMR was consistent with literature data.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,927-74-2, 3-Butyn-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; WANG, Bing, Hui; KRUM, Henry; SCAMMELLS, Peter; VINH, Natalie; SIMPSON, Jamie; CHALMERS, David; (148 pag.)WO2016/29263; (2016); A1;,
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Synthetic Route of 2566-44-1 ,Some common heterocyclic compound, 2566-44-1, molecular formula is C5H10O, 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 2-cyclopropylethanol at 0 C. (0.98 g, 11 mmol) and pyridine (2.4 mL, 30 mmol) in DCM (15 mL) was added 4-methylbenzene-1-sulfonyl chloride (22 g, 11 mmol). The cold bath was removed and the mixture allowed to warm to room temperature for 14 h. The reaction mixture was diluted with water and Et2O and the phases were separated. The organic phase was washed sequentially with water, 10% aqueous HCl and brine, dried (MgSO4) filtered and concentrated under reduced pressure to give Compound 4a (2.0 g, 74%) as a clear colorless oil. Compound 4a was used in the next step without further purification. MS m/z=241.4 (M+H). 1H NMR (400 MHz, chloroform-d) delta 7.77 (d, J=8.1 Hz, 2H), 7.32 (d, J=8.4 Hz, 2H), 4.06 (t, J=6.7 Hz, 2H), 2.42 (s, 3H), 1.56-1.45 (m, 2H), 0.70-0.57 (m, 1H), 0.44-0.32 (m, 2H), 0.04-0.10 (m, 2H).

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. 2566-44-1, 2-Cyclopropylethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; Pi, Zulan; Bilder, Donna M.; Brigance, Robert Paul; Finlay, Heather; Jiang, Wen; Johnson, James A.; Lawrence, R. Michael; Meng, Wei; Myers, Michael C.; Phillips, Monique; Tora, George O.; Zhang, Xiaojun; (59 pag.)US2017/275272; (2017); 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. 1072-52-2, name is 2-(Aziridin-1-yl)ethanol, molecular formula is C4H9NO, 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: 2-(Aziridin-1-yl)ethanol

(1) Preparation of 1-[2-(2-hydroxyethylamino)ethyl]-4-(4-nitrophenyl)piperazine (compound 75) In 20 ml of chloroform was dissolved 4 g of 1-(4-nitrophenyl)piperazine (compound 66) and 0.52 ml of 1-(2-hydroxyethyl)aziridine, and the solvent was distilled off from the resulting reaction mixture under reduced pressure. To the residue was added 10 mg of Amberlist 15 (trade name; made by Rohm & Haas Co.), and the mixture was then heated with stirring at 100 C. for 3 hour. Afterward, the temperature of the reaction mixture was returned to room temperature. To the reaction mixture was added 20 ml of chloroform, and insoluble matters were then removed therefrom by filtration. The filtrate was concentrated, and the resulting residue (concentrate) was purified through a silica gel column chromatograph (chloroform/methanol=100/1 to 25/1 in terms of volume ratio), thereby preparing 1 g of 1-[2-(2-hydroxyethylamino)ethyl]-4-(4-nitrophenyl)piperazine (compound 75).

With the rapid development of chemical substances, we look forward to future research findings about 1072-52-2.

Reference:
Patent; Mitsui Toatsu Chemicals, Incorporated; US5008267; (1991); A;,
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Electric Literature of 2919-23-5, 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 2919-23-5, name is Cyclobutanol. This compound has unique chemical properties. The synthetic route is as follows.

[CAS Reg. No. 1822782-90-0] DIAD (1.22 mL, 6.20 mmol) was added to a mixture of isoquinolin-6-ol (600 mg, 4.13 mmol), cyclobutanol (0.324 mL, 4.13 mmol) and PPh3 (1.63 g, 6.20 mmol) in anhyd THF (5 mL) at r.t. for 16 h. Additional PPh3 (1.63 g, 6.20 mmol) and DIAD (1.22 mL, 6.20 mmol) were added and the suspension was stirred at r.t. for a further 5 h. The mixture was loaded onto an SCX column; the column was first eluted with MeOH to remove by-products, then with 7 N ammonia in MeOH. Fractions containing the desired product were evaporated onto silica gel. The crude product was purified by flash silica gel chromatography (eluent: gradient 0 to 10% MeOH in CH2Cl2). Fractions containing the desired product were combined and evaporated to dryness to afford the title compound 29 (800 mg, 97%) as a yellow oil. MS (ES+): m/z = 200 [M + H]+.

According to the analysis of related databases, 2919-23-5, the application of this compound in the production field has become more and more popular.

Reference:
Article; Pearson, Stuart E.; Fillery, Shaun M.; Goldberg, Kristin; Demeritt, Julie E.; Eden, Jonathan; Finlayson, Jonathan; Patel, Anil; Synthesis; vol. 50; 24; (2018); p. 4963 – 4981;,
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Application of 2566-44-1, 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. 2566-44-1, name is 2-Cyclopropylethanol, molecular formula is C5H10O, 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.

The head space above a mixture of di-tert-butyl [(lr,4r)-6′-bromo-4-methoxy-5″-methyl-3’H- dispiro[cyclohexane-l,2′-indene-l’,2″-imidazol]-4″-yl]imidodicarbonate (Intermediate 9, 210 mg, 0.36 mmol), di-tert-butyl(2′,4′,6′-triisopropyl-3-methoxy-6-methylbiphenyl-2-yl)phosphine (10 mg, 0.02 mmol), allylpalladium chloride dimer (2.7 mg, 7.3 muiotaetaomicron), cesium carbonate (178 mg, 0.55 mmol) and 2-cyclopropylethanol (63 mg, 0.73 mmol) was evacuated and refilled with argon. Toluene (1.3 mL) was added and the mixture was heated at 90 C for 3 days. After another two days at r.t. the reaction mixture was filtered through a syringe filter. The filter was washed with 7 M ammonia in methanol (1.56 mL, 10.9 mmol). More 7 M ammonia in methanol (1.56 mL, 10.9 mmol) was added and the resulting solution was heated at 85 C for 24 h. After cooling to r.t. the mixture was concentrated. The residue was partitioned between EtOAc and 2 M aq. citric acid. The phases were separated and the organic layer was extracted twice with 2 M aq. citric acid. The organic layer was discarded. The aqueous citric acid phases were basified with NaOH (50% aq.) and extracted twice with EtOAc. The organic phase was treated with active charcoal, dried (Na2S0 ), filtered through diatomaceous earth and concentrated. Purification by flash silica gel chromatography, using a gradient of CHC^/MeOH (20: 1-15: 1-10: 1) gave the title compound (56 mg, 40% yield). 1H NMR (500 MHz, DMSO- ) delta ppm 0.02 – 0.12 (m, 2 H), 0.34 – 0.45 (m, 2 H), 0.72 – 0.84 (m, 1 H), 0.90 (td, 1 H), 1.07 – 1.27 (m, 2 H), 1.35 – 1.48 (m, 3 H), 1.53 (q, 2 H), 1.80 (d, 2 H), 2.15 (s, 3 H), 2.81 – 2.88 (m, 1 H), 2.88 – 2.98 (m, 2 H), 3.18 (s, 3 H), 3.80 – 3.91 (m, 2 H), 6.06 (d, 1 H), 6.50 (s, 2 H), 6.71 (dd, 1 H), 7.15 (d, 1 H); MS (ES+) m/z 382.1 [M+H]+.

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 2566-44-1, 2-Cyclopropylethanol.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; KARLSTROeM, Sofia; SOeDERMAN, Peter; SWAHN, Britt-Marie; Laszlo, Rakos; OeHBERG, Liselotte; WO2013/190301; (2013); A1;,
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Synthetic Route of 96-35-5, 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 96-35-5, name is Methyl 2-hydroxyacetate. This compound has unique chemical properties. The synthetic route is as follows.

To a suspension of KOtBu (996.6 mg, 8.881 mmol) in THF (640.4 mg, 8.881 mmol) cooled to 0 C was added dropwise methyl 2-hydroxyacetate (675.7 mu, 8.881 mmol) and stirred for 10 minutes. The acrylonitrile (589.1 mu, 8.881 mmol) was then added and the reaction stirred at ambient temperature. After 3 hours, the reaction was diluted with H20 (50 mL), then extracted with Et20 (25 mL) to remove any starting ester. The basic aqueous phase was acidified with 2M HC1 (5 mL), then extracted with Et20 (2 x 50 mL). The combined organic phases were dried with MgS04, filtered, and concentrated to afford a light brown oil (446 mg, 45.2% yield). 1H NMR (CDC13) delta 4.63 (t, 1H), 4.24 (t, 1H), 4.14 (d, 1H), 4.02 (d, 1H), 3.57 (t, 1H).

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 96-35-5, Methyl 2-hydroxyacetate.

Reference:
Patent; ARRAY BIOPHARMA INC.; ALLEN, Shelley; BLAKE, James F.; BRANDHUBER, Barbara J.; JIANG, Yutong; KOLAKOWSKI, Gabrielle R.; XU, Rui; WINSKI, Shannon L.; WO2014/78328; (2014); A1;,
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Synthetic Route of 4415-82-1, 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 4415-82-1 as follows.

To a suspension of sodium hydride (60% dispersion in mineral oil, 37 mg, 0.93 mmol) in THF (1 mL) was added cyclobutanemethanol (86 mu^, 0.91 mmol) at room temperature. A solution of compound 94 (200 mg, 0.46 mmol) in THF (3.5 mL) was added at room temperature. The mixture was stirred at room temperature for 30 min, at 50 C for 2 h, and cooled to room temperature. Aq. sat. NaHCCb was added. The mixture was extracted with EtOAc. The organic extract was dried withNa2SC>4, and concentrated. The residue was purified by flash chromatography (silica gel, eluting with 0% to 50% EtOAc in hexanes) to give compound 213 (203 mg, 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,4415-82-1, its application will become more common.

Reference:
Patent; REATA PHARMACEUTICALS, INC.; JIANG, Xin; BENDER, Christopher, F.; VISNICK, Melean; HOTEMA, Martha, R.; SHELDON, Zachary, S.; LEE, Chitase; CAPRATHE, Bradley, William; BOLTON, Gary; KORNBERG, Brian; (497 pag.)WO2018/111315; (2018); A1;,
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