Month: November 2020

2854-16-2 , The common heterocyclic compound, 2854-16-2, name is 1-Amino-2-methylpropan-2-ol, 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.

A dichloromethane (0.5 mL) solution of 1-(3-(cyclopropylcarbamoyl)-8-((4-methoxybenzyl)(methyl)ammno)imidazo[ 1 ,2-bj pyridazin-6-yl)- 1 H-indole-3-carboxylicacid (15 mg, 0.029 mmol), 1-amino-2-methylpropan-2-ol (7.86 mg, 0.088 mmol), N,NDiisopropylethylammne (0.026 mL, 0.147 mmol), and HATU (16.76 mg, 0.044 mmol)was stirred at room temperature. After 15 minutes the reaction became a clear brown solution, and was complete. It was concentrated to an oil, then loaded onto a 4g ISCO column for purification by flash chromatography, eluting with 0-100percent ethyl acetate inhexanes. The reaction afforded N-cyclopropyl-6-(3-((2-hydroxy-2-methylpropyl)carbamoyl)- 1H-indol- 1 -yl)-8-((4-methoxybenzyl)(methyl)amino)imidazo[1,2-bjpyridazine-3-carboxamide (17 mg, 0.026 mmol, 90percent yield) as a white solid. LC retention time 0.92 mm [Al. MS (ES+) m/z: 582 (MH).

The synthetic route of 2854-16-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; WEINSTEIN, David S.; DUNCIA, John V.; SPERGEL, Steven H.; (76 pag.)WO2018/93968; (2018); A1;,
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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 612-16-8 as follows., 612-16-8

General procedure: The solution of ionic-liquid-supported DMI 7 (2.2 mmol) in[bmim]PF6 (2 mL) was added to oxalyl chloride (2.0 mmol), andthe mixture was stirred at 60 C for 2 h. The mixture was then added to the appropriate alcohol (1.5 mmol), and the resultingmixture was stirred at r.t. overnight. Finally, the mixture wasextracted with hexane 10 mL x 3, and the organic layer wasconcentrated.

The chemical industry reduces the impact on the environment during synthesis 612-16-8, I believe this compound will play a more active role in future production and life.

Reference:
Article; Koguchi, Shinichi; Shibuya, Yuga; Igarashi, Yusuke; Takemura, Haruka; Synlett; vol. 30; 8; (2019); p. 943 – 946;,
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558-42-9, Adding a certain compound to certain chemical reactions, such as: 558-42-9, 1-Chloro-2-methyl-2-propanol, 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, 558-42-9, blongs to alcohols-buliding-blocks compound.

Example 7A 1-Chloro-2-methylpropan-2-yl {4,6-diamino-2-[1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]pyrimidin-5-yl}carbamate 175 mul (1.713 mmol) of 1-chloro-2-methyl-2-propanol were initially charged in 6 ml of dichloromethane, 169 mg (0.571 mmol) of bis(trichloromethyl) carbonate were added and the mixture was cooled to 0¡ã C. Thereafter, 110 mul (1.37 mmol) of pyridine were added dropwise and the mixture was stirred at 0¡ã C. for 30 min. Subsequently, 400 mg (1.142 mmol) of the compound from example 1A were added, and then 2.93 ml (36.26 mmol) of pyridine. The mixture was stirred at 0¡ã C. for a further 30 min. Then a separate flask was initially charged with 87 mul (0.856 mmol) of 1-chloro-2-methyl-2-propanol in 3 ml of dichloromethane, and 85 mg (0.285 mmol) of bis(trichloromethyl) carbonate were added. After adding 55 mul (0.685 mmol) of pyridine, the mixture was stirred at 0¡ã C. for 30 min and the solution thus prepared was added to the mixture described above. After stirring at 0¡ã C. for a further 30 min, the reaction was stopped by addition of 10 ml of saturated aqueous sodium hydrogencarbonate solution and extracted three times with dichloromethane. The combined organic phases were dried with sodium sulfate and concentrated under reduced pressure. This gave 500 mg (84percent of theory) of the title compound, which were used without further purification in the subsequent experiments. LC-MS (method 2): Rt=0.86 min; MS (EIpos): m/z=485 (M+H)+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,558-42-9, its application will become more common.

Reference:
Patent; BAYER INTELLECTUAL PROPERTY GMBH; Follmann, Markus; Stasch, Johannes-Peter; Redlich, Gorden; Ackerstaff, Jens; Griebenow, Nils; Knorr, Andreas; Wunder, Frank; Li, Volkhart Min-Jian; Baerfacker, Lars; Weigand, Stefan; US2014/148433; (2014); A1;,
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349-95-1, 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. 349-95-1, name is (4-(Trifluoromethyl)phenyl)methanol. A new synthetic method of this compound is introduced below.

B. Into another reactor, the concentration is 35%Aqueous hydrochloric acid 150kg and p-trifluoromethyl benzyl alcohol 50kg,Stir and heat to reflux, keep reaction for 24h,Cool to room temperature, layer, take organic layer,Dehydrated with anhydrous sodium sulfate,Distillation under vacuum gives a pairTrifluoromethyl benzyl chlorideThe content is 98.8%. Step B of equation (2) is as follows:

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. 349-95-1, (4-(Trifluoromethyl)phenyl)methanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Jiangsu Bandung Technology Co., Ltd.; Wu Yongcai; (5 pag.)CN107793292; (2018); A;,
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355-80-6, 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. 355-80-6, name is 2,2,3,3,4,4,5,5-Octafluoro-1-pentanol. A new synthetic method of this compound is introduced below.

General rocedure: 5.5 ml of aq. solutions of KBr (0.55 mol/dm3), 20 ml MeCN, TEMPO (0.12 g, 0.00077 mol), and 2,2,3-trifluoro-3-(1,1,2,2,3,3-hexafluoro-3-trifluoromethoxy-propoxy)-propan-1-ol (2a) (10 g, 0.0275 mol) were placed in the flask. 14% aq. NaOCl (48 ml) buffered by NaHCO3 (5.2 g) were added via the dropping funnel in 3 portions during two days of stirring in a room temperature (slight exothermic effect). The progress of reaction was monitored by 19F NMR spectroscopy. Then concentrated sulfuric acid followed by water was added. After extraction with diethyl ether, the organic phases were dried over magnesium sulfate. The solvent was evaporated to give a colorless liquid, which was distilled.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,355-80-6, 2,2,3,3,4,4,5,5-Octafluoro-1-pentanol, and friends who are interested can also refer to it.

Reference:
Article; Ignatowska, Jolanta; Shyshkov, Oleg; Zipplies, Tilman; Hintzer, Klaus; Roeschenthaler, Gerd-Volker; Journal of Fluorine Chemistry; vol. 141; (2012); p. 35 – 40;,
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Adding some certain compound to certain chemical reactions, such as: 3973-18-0, name is Propynol ethoxylate, 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 3973-18-0. 3973-18-0

A solution of 1.7 g of lib and 3 ml of triethyl amine in 20 ml of diethyl ether was treated at O0C with 1.5 ml of methanesulfonyl chloride. The mixture was stirred for an additional 30 min and then diluted with 35 ml of water and extracted with ethyl acetate. The combined organic layers were washed with IM aq. K2CO3 solution and water, dried and concentrated, to provide 2.45 of lie as a colorless oil; Rf 0.45 (heptane/ethyl acetate 1/1).NMR (CDCl3) delta 2.48 (t, 1, acetylene-H), 3.08 (s, 3, CH3SO2), 3,82 (m, 2, CH2), 4.03( d, 2, CH2), 4.41 (m, 2, CH2).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 3973-18-0.

Reference:
Patent; N.V. ORGANON; LOOZEN, Hubert, Jan, Jozef; TIMMERS, Cornelis, Marius; STOCK, Herman, Thijs; WO2011/12600; (2011); A1;,
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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. 455-01-6, name is 2-(3-(Trifluoromethyl)phenyl)ethanol, the common compound, a new synthetic route is introduced below. 455-01-6

General procedure: DIAD (0.65mL, 3.31mmol) was added dropwise to 12a or 12b (500mg, 2.21mmol), PPh3 (869mg, 3.31mmol) and appropriate alcohol [2-phenylethanol (0.27mL, 2.21mmol, 2e; or 0.17mL, 1.46mmol, 2k), 2-(3-methoxyphenyl)ethanol (0.31mL, 2.21mmol, 2f; 0.20mL, 1.46mmol, 2l), or 2-(3-trifluoromethylphenyl)ethanol (0.33mL, 2.21mmol, 2g and 2m] in THF (10mL), and the mixture was stirred for 18h. Drying, evaporation and chromatography (PE/EtOAc 20:1) gave the esters 2e-g, k-m. Spectroscopic data for these compounds are given in the Supporting information.

Statistics shows that 455-01-6 is playing an increasingly important role. we look forward to future research findings about 2-(3-(Trifluoromethyl)phenyl)ethanol.

Reference:
Article; Yevglevskis, Maksims; Nathubhai, Amit; Wadda, Katty; Lee, Guat L.; Al-Rawi, Suzanne; Jiao, Tingying; Mitchell, Paul J.; James, Tony D.; Threadgill, Michael D.; Woodman, Timothy J.; Lloyd, Matthew D.; Bioorganic Chemistry; vol. 92; (2019);,
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1777-82-8, 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. 1777-82-8, name is (2,4-Dichlorophenyl)methanol, molecular formula is C7H6Cl2O, 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.

General procedure: 0.5 mmol substrate, 1.5 mmol NH4OAc, 0.15 mmol TEMPO, 2 mL AcOH and 0.15 mmol HNO3 weresuccessively added to a dried 45 mL tube filled with 1atm oxygen. Then the reaction tube was sealed andplaced in a constant-temperature oil bath to perform the reaction for 12 h. Once the reaction time wasreached, the mixture was cooled to room temperature. Then the mixture was alkalized to pH 7-8 with sodiumhydroxide aqueous solution. GC analysis of organic phase provided the GC yields of the products.Subsequently, the crude product from another parallel experiment was purified by column chromatography,and identified by 1H-NMR, 1C-NMR or GC-MS

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. 1777-82-8, (2,4-Dichlorophenyl)methanol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Zhao, Bo; Ren, Yun-Lai; Ren, Fangping; Tian, Xinzhe; Zhao, Shuang; Letters in Organic Chemistry; vol. 15; 7; (2018); p. 627 – 632;,
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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. 6338-55-2, name is 2-(2-(2-Aminoethoxy)ethoxy)ethanol. This compound has unique chemical properties. The synthetic route is as follows. 6338-55-2

A solution of the amino alcohol (620) (313.6 g, 2.1mol) in THF (3.5 L) was treated, portion- wise, with N-(Benzyloxycarbonyloxy)succinimide (621) (550 g, 2.21mol). Once the reaction was complete (18 h) the THF was removed under reduced pressure and the residue dissolved in CH2Cl2 (2.5 L), then washed with an equal volume of HCl (1 M), NaHCO3 (Sat. Aq.), H2O and brine. The organic extract was dried (MgSO4), filtered and concentrated. The crude material (600g) was subjected to chromatography (4kg silica; 1-12% CH3OH-CH2Cl2) to yield HO- Trig-NHZ (622) (468g, 78%) as a clear-yellow viscous oil.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,6338-55-2, 2-(2-(2-Aminoethoxy)ethoxy)ethanol, and friends who are interested can also refer to it.

Reference:
Patent; GENEVANT SCIENCES GMBH; HEYES, James; HOLLAND, Richard J.; JUDGE, Adam; LAM, Kieu Mong; (0 pag.)WO2020/93061; (2020); A1;,
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2615-15-8, 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 2615-15-8, name is 3,6,9,12,15-Pentaoxaheptadecane-1,17-diol. This compound has unique chemical properties. The synthetic route is as follows.

Step 1.In a 50 mL three-necked flask, add TsCl (6.05 g, 31.9 mmol),Hexaethylene glycol (3.81 g, 12.8 mmol), a catalytic amount of 4-dimethylaminopyridine (20 mg) and 20 mL of CH2Cl2,Under an ice-salt bath, triethylamine (6.55 g, 64.8 mmol) was added dropwise using a constant pressure dropping funnel.After stirring at room temperature for 12h, the reaction was stopped and washed with 1M HCl solution (30mL ¡Á 3).Wash with saturated sodium bicarbonate solution (30 mL ¡Á 3), wash with saturated brine (30 mL ¡Á 3), and dry with anhydrous sodium sulfate. Filter and spin dry.Column chromatography separation: CH2Cl2 ? CH2Cl2: EA = 1: 1, red compound A was obtained as a viscous liquid.

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 2615-15-8, 3,6,9,12,15-Pentaoxaheptadecane-1,17-diol.

Reference:
Patent; Changzhou University; Xiao Tangxin; Zhou Ling; Wu Kehui; Li Zhengyi; Sun Xiaoqiang; (6 pag.)CN110372682; (2019); A;,
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