Tag: M.W=0-100

Adding a certain compound to certain chemical reactions, such as: 2867-59-6, 3-Aminobutan-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, 2867-59-6, blongs to alcohols-buliding-blocks compound. category: alcohols-buliding-blocks

Add 250.0g of absolute ethanol and 110.5g of 4-hydroxy-2-butanone to a 1L reaction flask. 85.3g of NH3 was passed in at 10 C. The reaction solution was transferred to an autoclave, and 8.0 g of Raney nickel was added.Nitrogen and hydrogen were replaced three times, pressurized to 1.3MPa with hydrogen, the mixture was stirred at 45 C for 20 hours. GC detection of 4-hydroxy-2-butanol was less than 1.0%. The product was filtered and concentrated under reduced pressure at 45 C in a water bath. The concentrated solution was dissolved in toluene and stirred at 110 C. for 4 hours. Water was separated to obtain a lower layer. After concentrating again in a water bath at 50 C, distillation under reduced pressure of -0.9 MPa was performed, and a fraction of 80-120 C was received. The fraction was diluted with 40 g of absolute ethanol, add dropwise to a 500ml reaction bottle containing 85.2g of absolute ethanol and 65.0g of L-mandelic acid. The solution was added dropwise for 1 hour and maintained at a temperature of 55 C, and then reacted at 75 C for 20 minutes. The temperature was slowly lowered for 24 hours to 12 C, a solid was precipitated and filtered to obtain a crude filter cake. Stir the crude product with 250.8 g of isopropanol at 85 C and slowly reduce the temperature to 13 C for 3 hours. Filter again to get a crude filter cake. The above-mentioned operation of beating crystal filtration was repeated three times in total. Drying gave 80.6 g of constant weight white crystals. A 250 ml reaction tank was charged with 60.0 g of methanol, 80.6 g of white crystals, and 56.4 g of a 30% sodium methoxide methanol solution. The reaction was refluxed at 65 C for 17 hours. The temperature was lowered to 3 C and stirred for 30 minutes. Filtration at 3 C and concentration at 37 C were repeated twice to obtain 43.0 g of a colorless liquid. Distillate under reduced pressure at 125 C and receive 80-120 C fractions. Yield: 28.0%, GC: 99.9%, ee value is greater than 99.9%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,2867-59-6, its application will become more common.

Reference:
Patent; Jiangsu Baoli Chemical Co., Ltd.; Li Yiqing; Li Zhenqi; Li Tianxin; (9 pag.)CN110668958; (2020); A;,
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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 2516-33-8, name is Cyclopropylmethanol. This compound has unique chemical properties. The synthetic route is as follows. SDS of cas: 2516-33-8

Intermediate 1:Preparation of cyclopropylmethyl 2,5-dioxopyrrolidin-l-yl carbonate. added bis(2,5-dioxopyrrolidin-l -yl) carbonate (7.1 g, 27.7 mmol) and triethylamine (5.8 mL, 41.6 mmol). The reaction was stirred overnight then quenched with saturated NaHC03 (aq.) and extracted with ethyl acetate (3 chi 50 mL), dried over sodium sulfate, filtered and concentrated under reduced pressure to provide the title compound as an amber oil: NMR (300 MHz, CDC13) delta 4.16 (d, J = 7.5 Hz, 2H), 2.84 (s, 4H), 1.26 (m, 1H), 0.70-0.64 (m, 2H), 0.40-0.35 (m, 2H).

With the rapid development of chemical substances, we look forward to future research findings about 2516-33-8.

Reference:
Patent; MERCK SHARP & DOHME CORP.; EDMONDSON, Scott; GUO, Zhiqiang; GEISS, William, B.; WOOD, Harold, B.; STAMFORD, Andrew, W.; MILLER, Michael, W.; DEMONG, Duane, E.; MORRIELLO, Gregori, J.; ANAND, Rajan; COLANDREA, Vincent, J.; MACALA, Megan; MALETIC, Milana; ZHU, Cheng; ZHU, Yuping; SUN, Wanying; ZHAO, Kake; HUANG, Yong; HARRIS, Joel, M.; CHANG, Lehua; KAR, Nam Fung; HU, Zhiyong; WANG, Liping; WANG, Bowei; LIU, Ping; SZEWCZYK, Jason, W.; WO2012/138845; (2012); A1;,
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Adding a certain compound to certain chemical reactions, such as: 3513-81-3, 2-Methylenepropane-1,3-diol, 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, 3513-81-3, blongs to alcohols-buliding-blocks compound. HPLC of Formula: C4H8O2

To a solution of di-tert-butyl dicarbonate (6.6 kg) in methylene chloride (15.0 L, 15 volumes) was added 2-methylene-1,3-propanediol (1.00 kg) and phase transfer catalyst tetrabutylammonium hydrogensulfate (0.641 kg). The resulting reaction mixture was then agitated vigorously at about 15° C. while adding over a 2 hr period, 6M aqueous sodium hydroxide solution (13.2 L) and controlling the temperature between 25 to 30° C. The resulting two-phase reaction mixture was subsequently agitated for a period of 2-3 hrs at 25° C.The aqueous layer was discarded and additional phase transfer catalyst tetrabutylammonium hydrogensulfate (0.064 kg, 10percent of the initial amount), di-tert-butyl dicarbonate (0.66 kg, 10percent of the initial amount), and methylene chloride (2.0 L, 2 volumes) was added to the remaining organic reaction mixture. To the reaction mixture was also added 6M aqueous sodium hydroxide solution (1.32 L, 10percent of the initial amount) over a period of about 0.5 to 1 hr, while controlling the temperature between 25 to 30° C. The resulting two-phase reaction mixture was then agitated at about 25° C. for additional 3 to 4 hr. Allowing more than 3 hrs of agitation time is often required to complete the hydrolysis of the excess di-tert-butyl dicarbonate. The aqueous layer was discarded. The resulting organic phase was washed with water (3.x.8.0 L), diluted with EtOAc (6 L, 6 volumes), and distilled to an oil foam with quantitative yield.1H (500 MHz, CDCl3) delta 5.15, 4.98, 4.79, 4.68, 4.68, 4.33, 4.31, 3.89, 3.77, 3.67, 3.45, 3.35, 3.19, 2.88, 2.78, 2.74, 2.42, 2.17, 2.11, 2.06, 1.95, 1.72, 1.66, 1.51, 1.48, 1.43, 1.34, 1.27, 1.19, 1.19, 1.18, 1.14, 1.13, 1.11, 0.95, 0.85.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,3513-81-3, its application will become more common.

Reference:
Patent; Xu, Guoyou; Gai, Yonghua; Wang, Guoqlang; Or, Yat Sun; Wang, Zhe; US2007/207972; (2007); A1;,
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Electric Literature of 2867-59-6 ,Some common heterocyclic compound, 2867-59-6, molecular formula is C4H11NO, 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.

2-(3-Fluorophenyl)-3-oxo-6-[4-(trifluorom acid (100 mg, 0.26 mmol) was dissolved in anhydrous DMF (2.0 ml_). (3RS)-3-Aminobutan-1 -ol (47.1 mg, 0.53 mmol), N-ethyl-N-isopropylpropan-2-amine (0.207 ml_, 1.19 mmol), and propane phosphonic acid anhydride (T3P, 231 muIota_, 50% in DMF, 397 muetaiotaomicronIota) were successively added. It was stirred at rt overnight. The crude reaction mixture was purified by RP-HPLC (column: X-Bridge C18 5muetaiota 100x30mm, mobile phase: (water + 0.1 vol% formic acid (99%)) / acetonitrile, gradient) to yield 88.3 mg (74%) of the title compound. 1H-NMR (400MHz, DMSO-d6): delta [ppm] = 1 .19 (d, 3H), 1.60 – 1.74 (m, 2H), 3.45 – 3.51 (m, 2H), 4.09 – 4.21 (m, 1 H), 4.51 (t, 1 H), 7.36 – 7.43 (m, 1 H), 7.54 – 7.58 (m, 1 H), 7.59 – 7.66 (m, 2H), 7.88 (d, 2H), 8.20 (d, 2H), 8.70 (s, 1 H), 9.29 (d, 1 H).

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. 2867-59-6, 3-Aminobutan-1-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; DEUTSCHES KREBSFORSCHUNGSZENTRUM (DKFZ); SCHMEES, Norbert; GUTCHER, Ilona; IRLBACHER, Horst; BADER, Benjamin; ZHAO, Na; PLATTEN, Michael; (437 pag.)WO2017/202816; (2017); A1;,
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Application of 1589-47-5, 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. 1589-47-5, name is 2-Methoxypropan-1-ol. A new synthetic method of this compound is introduced below.

The distillate of example 2 was dewatered by means of azeotropic distillation using a distillation column having an inner diameter of 25 mm and a filling with stainless steel coils. The column had a separation efficiency of 25 theoretical stages and was equipped with external electric heating to compensate heat loss. The distillate of example 2 was fed continuously at a rate of 150 g/h to the 3rd theoretical stage (counted from the top) of said column. Additionally benzene was fed to the top of the column. The reboiler was heated to obtain 1235 g/h distillate. The distillate was condensed and transferred to a phase separation vessel, in that it separated to a benzene phase and an aqueous phase. The benzene phase was again fed to the top of the column and the aqueous phase was removed at a rate of 115 g/h. Simultaneously, a bottom product was removed at a rate of 35 g/h. The content of organic compounds of the bottom product was analyzed via gc-analysis. The water content was determined by Karl-Fischer-Titration.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,1589-47-5, 2-Methoxypropan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; DEGUSSA AG; UHDE GMBH; WO2004/773; (2003); A1;,
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Adding a certain compound to certain chemical reactions, such as: 2516-33-8, Cyclopropylmethanol, 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

General procedure: To a solution of (3,3-difluorocyclobutyl)methanol (4.0 g, 32.8 mmol) in dichloromethane (109 ml) at room temperature was added Dess-Martin Periodinane (16.7 g, 39.3 mmol). After 2 h, the reaction was diluted with two volumes of ether and treated with sodiumthiosulfate (32 g) in water (160 mL). After stirring at room temperature for 10 min, the layers were separated. The ethereal was washed with saturated sodium bicarbonate (2X), dried over magnesium sulfate, and filtered. The resulting solution was concentrated via distillation of the solvent through a short path distillation apparatus. The distillation was discontinued when 6.56 g remained in the boiling flask. Integration of the 1H NMR showed product as a 28.4 wt% solution in diethyl ether (1.86 g, 47% yield). The material was directly used without further concentration

The synthetic route of 2516-33-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Degnan, Andrew P.; Maxwell, Darrell; Balakrishnan, Anand; Brown, Jeffrey M.; Easton, Amy; Gulianello, Michael; Hanumegowda, Umesh; Hill-Drzewi, Melissa; Miller, Regina; Santone, Kenneth S.; Senapati, Arun; Shields, Eric E.; Sivarao, Digavalli V.; Westphal, Ryan; Whiterock, Valerie J.; Zhuo, Xiaoliang; Bronson, Joanne J.; Macor, John E.; Bioorganic and Medicinal Chemistry Letters; vol. 26; 24; (2016); p. 5871 – 5876;,
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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., Formula: C3H6O

Water (300 ml),Cyclopropanol (500 ml),N, N-diethyl-2,3,3,3-tetrafluoropropanamide (900 g, 4.47 mol),98% sulfuric acid (600 ml) was placed in the reaction flask,The temperature was raised to 130 C and refluxed for 12 hours.Reaction completed,Atmospheric distillation,Fractions of around 127 C were collected to give cyclopropyl 2,3,3,3-tetrafluoropropionate,The yield was 90%Purity 98.6%.

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; Zhao, Manliang; (9 pag.)CN106278887; (2017); A;,
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Reference of 534-03-2, 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. 534-03-2, name is 2-Aminopropane-1,3-diol. A new synthetic method of this compound is introduced below.

45.6 g of 2-amino-1,3-dihydroxypropane was mixed with 113 mL of formic acid solution,Then add 90 mL of 37% formaldehyde solution.The mixture was stirred at room temperature for 2h,The reaction was then warmed to 80 C,And kept at this temperature overnight.When the temperature reaches 80 , there will be a lot of gas discharge. After the reaction was completed, it was cooled to room temperature. 60 mL of 37% strength hydrochloric acid was added and stirred for 1 h.Solid sodium hydroxide was added to adjust the pH of the solution to 12, the mixture was distilled under reduced pressure,Add a lot of methanol.At this point the white precipitate generated in the system filter, the filtrate was distilled off under reduced pressure,The concentrated initial product was dissolved in trichloromethane and dried over anhydrous magnesium sulfate.In the conditions of 100 -102 / 100Kpa by distillation,40.9 g was obtained2-N, N-dimethyl-1,3-dihydroxypropane,The yield was 68.65%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,534-03-2, 2-Aminopropane-1,3-diol, and friends who are interested can also refer to it.

Reference:
Patent; University of Science and Technology Beijing; Gong Aijun; Yang Jing; Qiu Lina; Xie Yanping; Zhao Yunbo; (9 pag.)CN105198773; (2017); B;,
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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.

To a mixture of 2-cyclopropylethanol (5.35 g, 62.1 mmol) and dichloromethane (107 mL) were added methanesulfonyl chloride (5.29 mL, 68.3 mmol) and triethylamine (13.1 mL, 93.1 mmol) in that order while stirring on ice, and the resulting mixture was stirred for 1 hour. Water and ethyl acetate were then added to the reaction mixture. After thoroughly shaking the mixture, the organic layer was separated and the organic layer was washed with brine and dried over anhydrous magnesium sulfate. The mixture was then filtered, and the solvent in the filtrate was distilled off under reduced pressure to obtain the title compound (10.3 g, 62.7 mmol). 1H-NMR (CDCl3) delta: 0.10-0.16 (m, 2H), 0.48-0.55 (m, 2H), 0.72-0.83 (m, 1H), 1.65 (q, J=6.8 Hz, 2H), 3.01 (s, 3H), 4.29 (t, J=6.8 Hz, 2H).

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; Eisai R & D Management Co., Ltd.; US2009/259049; (2009); A1;,
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Electric Literature of 2566-44-1, 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. 2566-44-1, name is 2-Cyclopropylethanol. A new synthetic method of this compound is introduced below.

General procedure: Example 5-01 (Typical Procedure 10) [0342] A mixture of (R)-3-(2-bromo-pyridin-4-yloxy)-1-(7-fluoro-3-oxo-indan-5-yl)-pyrrolidin-2-one (80 mg), 2-cyclopropyl-ethanol (85 mg), cesium carbonate (129 mg) and toluene (1.6 mL) under argon was added Pd(OAc)2 (443 mug) and 5-(di-tert-butylphosphino)-1?,3?,5?-triphenyl-1?H-[1,4?]bipyrazole (2.0 mg). The mixture was heated to 90 C. for 2 hours by microwave irradiation. After cooling to room temperature the mixture was filtered and concentrated. The residue was purified by preparative HPLC to provide Example 5-01.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,2566-44-1, its application will become more common.

Reference:
Patent; SANOFI; SCHWINK, Lothar; BOSSART, Martin; GLOMBIK, Heiner; GOSSEL, Matthias; KADEREIT, Dieter; KLABUNDE, Thomas; MAIER, Thomas; STENGELIN, Siegfried; US2014/99333; (2014); A1;,
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