Category: 2568-33-4

Electric Literature of 2568-33-4, Adding some certain compound to certain chemical reactions, such as: 2568-33-4, name is 3-Methylbutane-1,3-diol,molecular formula is C5H12O2, 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 2568-33-4.

The 3 – methyl – 1, 3 butanediol (14 A) (5.0 g, 48 mmol) dissolved in dichloromethane (100 ml) in, add triethylamine (9.7 g, 96 mmol), 0 C slow […] carboxylic acid isopropyl ester (8.8 g, 72 mmol), transfusion reaction at room temperature for 3 hours. The reaction solution by adding water (100 ml) washing, for liquid phase after the saturated salt water (100 ml × 1) washing, drying with anhydrous sodium sulfate, filtered, the filtrate is concentrated under reduced pressure, the residue with silica gel column chromatography (ethyl acetate/petroleum ether (v/v)=1/10 – 1/1) separating and purifying, to obtain the title compound (3 – hydroxy -3 – methyl – butyl) isopropyl carbonate (14 B), colorless oily matter (4.5 g, yield 49%).

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. 2568-33-4, 3-Methylbutane-1,3-diol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Sichuan Hai Sike Pharmaceutical Co., Ltd.; Qiu Guanpeng; Wei Yonggang; Lu Yonghua; Huang Qingping; Liao Pengfei; (41 pag.)CN107382870; (2017); A;,
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Related Products of 2568-33-4, 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 2568-33-4, name is 3-Methylbutane-1,3-diol. This compound has unique chemical properties. The synthetic route is as follows.

Step 1. Preparation of 3-hydroxy-3-methylbutyl 4-methylbenzenesulfonate To a solution of 3-methylbutane-l,3-diol (1.00 g, 9.60 mmol) in pyridine (10 mL) at 0 C was added -toluenesulfonyl chloride (2.014 g, 10.56 mmol). The reaction mixture was stirred for 16 h while allowing the reaction mixture to slowly warm up to room temperature by dissipation of the ice-water bath. The mixture was transferred to a separatory funnel containing ethyl acetate (100 mL). The organic layer was washed with 1 N HQ (3 x 50 mL). The organic layer was then washed with saturated aHC03 solution (50 mL), brine (50 mL), dried over MgS04, filtered, and concentrated. The product was purified by column chromatography on silica gel (30%? 50% ethyl acetate in hexanes; 220 g column) to afford 3-hydroxy-3-methylbutyl 4-methylbenzenesulfonate (2.03 g, 7.86 mmol, 82% yield) as a colorless oil: XH NMR (400MHz, CHLOROFORM- d) delta 7.85 – 7.78 (m, 2H), 7.37 (dd, J=8.5, 0.8 Hz, 2H), 4.23 (t, J=6.9 Hz, 2H), 2.47 (s, 3H), 1.88 (t, J=6.9 Hz, 2H), 1.24 (s, 6H); LC/MS: The product did not ionize, tR = 1.78 min (method 2-1).

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 2568-33-4, 3-Methylbutane-1,3-diol.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; SIT, Sing-Yuen; CHEN, Yan; CHEN, Jie; SWIDORSKI, Jacob; VENABLES, Brian Lee; SIN, Ny; MEANWELL, Nicholas A.; REGUEIRO-REN, Alicia; HARTZ, Richard A.; XU, Li; LIU, Zheng; WO2015/157483; (2015); A1;,
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Related Products of 2568-33-4, 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. 2568-33-4, name is 3-Methylbutane-1,3-diol, molecular formula is C5H12O2, 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.

Step 1: 3-Hydroxy-3-methylbutyl 4-methylbenzenesulfonate To a solution of 3-methylbutane-1,3-diol (2.5 mL) in dichloromethane (30 mL) and pyridine (2.1 mL) is added at 0 C. p-toluene-sulfonylchloride (4.6 g) in portions. The mixture is stirred for 12 hours at room temperature, diluted with dichloromethane and washed with 1 M aqueous HCl solution and brine. After drying (MgSO4) the solvent is evaporated and the product is purified by chromatography on silica gel (cyclohexane/ethyl acetate 90:10?70:30) to give the title compound. Yield: 3.2 g; Mass spectrum (ESI+): m/z=276 [M+NH4]+.

According to the analysis of related databases, 2568-33-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Boehringer Ingelheim International GmbH; ECKHARDT, Matthias; FRATTINI, Sara; HAMPRECHT, Dieter; HIMMELSBACH, Frank; LANGKOPF, Elke; LINGARD, Iain; PETERS, Stefan; WAGNER, Holger; US2013/252937; (2013); A1;,
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Electric Literature of 2568-33-4 , The common heterocyclic compound, 2568-33-4, name is 3-Methylbutane-1,3-diol, molecular formula is C5H12O2, 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 stirred solution of compound la (4 g, 38 mmol) in DMF (30 mL) was added NaH (3.3 g,8.4 mmol, 60% in mineral oil) at 0C over 10 mins. The mixture was stirred for half an hour atr.t., and then cooled to 0 C. Then compound 7-1 (6 g, 32 mmol) in DMF (20 mL) was added to5 the reaction, and the reaction was stirred at r.t. for 12 h. The reaction was poured into water(100 mL), and the resulting mixture was stirred for 10 min. The mixture was then was extractedwith EtOAc (60 mL x 3). The organic layers were combined, washed with water (60 mL), brine( 60 mL ), dried and concentrated to give crude product, which was used directly for the next stepwithout further purification. MS (ESI) m/z: 274.1.

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

Reference:
Patent; MERCK SHARP & DOHME CORP.; HAGMANN, William K.; NARGUND, Ravi P.; BLIZZARD, Timothy A.; JOSIEN, Hubert; BIJU, Purakkattle; PLUMMER, Christopher W.; DANG, Qun; LI, Bing; LIN, Linus S.; CUI, Mingxiang; HU, Bin; HAO, Jinlai; CHEN, Zhengxia; WO2014/19186; (2014); A1;,
Alcohol – Wikipedia,
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Reference of 2568-33-4, Adding some certain compound to certain chemical reactions, such as: 2568-33-4, name is 3-Methylbutane-1,3-diol,molecular formula is C5H12O2, 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 2568-33-4.

A 50 mL three-necked flask that had been equipped with a column fitted with a side tube and packed with 20 g of molecular sieve (4A), a condenser, a thermometer and a drying tube was loaded with 0.64 g (2 mmol) of N, N?-bis(salicylidene)ethylenediamine iron (II), 1.04 g (10 mmol) of isoprene glycol, 40 g (400 mmol) of methyl methacrylate, 0.08 g of phenothiazine and 0.2 g of tridecane. While performing stirring at atmospheric pressure, the flask was placed into an oil bath set at 120 C. so that the temperature inside the flask would be 100 to 105 C. The reaction was performed for 11 hours while totally refluxing the distilled fraction back to the reaction system through the molecular sieve. The reaction liquid was sampled at prescribed lapses of time from the start of the reaction (3 hours, 5 hours, 7 hours, 9 hours and 11 hours). The gelation of the samples of the reaction liquid was evaluated as described in Test Example 3, the results being described in Table 1.

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. 2568-33-4, 3-Methylbutane-1,3-diol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; KURARAY CO., LTD.; TAKAHATA, Yusuke; KAJIYASHIKI, Tsuyoshi; (9 pag.)US2018/50975; (2018); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Reference of 2568-33-4, 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. 2568-33-4, name is 3-Methylbutane-1,3-diol, molecular formula is C5H12O2, 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.

Into a 1 L three-necked flask equipped with a stirrer, a dry air inlet tube, a thermometer, a distillation column (inner diameter 25 mm ¡Á height 300 mm, packing tower packed with 6 mm McMahon packing) and a distillation head,100 g of 3-methyl-3-hydroxy-1-butyl alcohol, 240 g of methyl methacrylate,0.24 g of 2,2,6,6-tetramethyl-4-hydroxypiperidine-N-oxide as a polymerization inhibitor was charged,While stirring while blowing a small amount of air,The inside of the system was heated to 100 to 110 C. 8 g of methyl methacrylate was withdrawn from the top portion of the distillation column. After cooling the inside of the system to 40 C., 0.55 g of magnesium diethoxide was charged as a catalyst, and a small amountWhile blowing air while stirring,The inside of the system was heated to 100 to 130 C. Methanol produced as the reaction proceeded was gradually withdrawn from the top of the distillation column by azeotropic distillation with methyl methacrylate to allow the reaction to proceed.The conversion of 3-methyl-3-hydroxy-1-butyl alcohol 7 hours after the start of the reaction was 78.3%. The reaction was further continued, and after 9 hours from the start of the reactionThe conversion of 3-methyl-3-hydroxy-1-butyl alcohol was 94.0%The yield of 3-methyl-3-hydroxy-1-butyl methacrylate based on 3-methyl-3-hydroxy-89.3%,The diester yield based on 3-methyl-3-hydroxy-1-butyl alcohol was 1.7%.

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 2568-33-4, 3-Methylbutane-1,3-diol.

Reference:
Patent; Mitsubishi Gas Chemical Company; Kushida, Eriko; Takemoto, Makiko; (16 pag.)JP2018/135285; (2018); A;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Adding a certain compound to certain chemical reactions, such as: 2568-33-4, 3-Methylbutane-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, HPLC of Formula: C5H12O2, blongs to alcohols-buliding-blocks compound. HPLC of Formula: C5H12O2

Example 2OC; N-r(2Z)-3-butviri.31thiazolor4.5-clpyridin-2(3H)-ylidenel-2-(3-hvdroxy-3-methylbutoxy)-5-(trifluoromethyl)benzamide; 3-Methylbutane-l,3-diol (42 mg, 0.4 mmol) in THF (1 mL) was treated with NaH (60%) (16 mg, 0.4 mmol) at room temperature for 20 min. To the above mixture, which was cooled to 0-5 0C, was added the product from Example 2OB (80 mg, 0.2 mmol) in THF (1 mL). After 20 min. the reaction mixture was quenched with saturated aqueous NaHCO3 (20 mL) and extracted with ethyl acetate (2 x 30 mL). The combined organic extracts were dried over anhydrous Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified by column chromatography using an Analogix Intelliflash280 (SiO2, 0-100 % ethyl acetate in hexanes) to afford 87 mg (90 %) of the title compound. 1H NMR (500 MHz, CDCl3) delta ppm 1.04 (t, J=7.32 Hz, 3 H) 1.36 (s, 6 H) 1.47 – 1.55 (m, 2 H) 1.88 – 1.96 (m, 2 H) 2.13 (t, J=5.80 Hz, 2 H) 4.35 (t, J=5.80 Hz, 2 H) 4.54 (t, J=7.63 Hz, 2 H) 5.12 (brs, 1 H) 7.11 (d, J=8.54 Hz, 1 H) 7.61 (d, J=5.19 Hz, 1 H) 7.74 (dd, J=8.54, 2.14 Hz, 1 H) 8.49 (d, J=5.19 Hz, 1 H) 8.68 (s, 1 H) 8.72 (s, 1 H); MS (ESI+) m/z 482 (M+H)+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2568-33-4, 3-Methylbutane-1,3-diol, and friends who are interested can also refer to it.

Reference:
Patent; ABBOTT LABORATORIES; FROST, Jennifer, M.; LATSHAW, Steven, P.; DART, Michael, J.; CARROLL, William, A.; PEREZ-MEDRANO, Arturo; KOLASA, Teodozyj; PATEL, Meena; NELSON, Derek, W.; LI, Tongmei; PEDDI, Sridhar; WANG, Xueqing; LUI, Bo; WO2010/71783; (2010); A1;,
Alcohol – Wikipedia,
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Application of 2568-33-4, Adding some certain compound to certain chemical reactions, such as: 2568-33-4, name is 3-Methylbutane-1,3-diol,molecular formula is C5H12O2, 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 2568-33-4.

General procedure: In the Schlenk reaction vessel,Methyltri n-octylphosphonium methyl carbonate([Me (n-octyl) 3P] + [OCO2Me]-,Charge the catalyst (C1a), 55.8 muL, 0.12 mmol),Methyl methacrylate (MMA, 4 mL) was added and stirred at room temperature for 1 to 2 minutes. Then, 3-methylbutane-1,3-diol (compound (3a), 21 3 muL, 2.0 mmol), internal standard substance (4,4′-di-tert-butylbiphenyl, 53.3 mg, 0.20 mmol), 1.0 g of dried powdery molecular sieves 5A (MS 5A) was added, and the mixture was stirred at room temperature (25 C.) for 3 hours to carry out an ester exchange reaction represented by the following formula. During the reaction, the progress of the reaction was confirmed by thin layer chromatography (TLC) as appropriate. The reaction mixture was passed through a celite pad to remove MS 5A, MMA was distilled off from the mixture under reduced pressure, and after concentration, the yield of the reaction product was measured by 1H NMR (internal standard method). The concentrate was subjected to silica gel column chromatography (n-hexane: ethyl acetate = 50: 1 to 10: 1) to isolate a carboxylic acid monoester (compound (4a)). The yield and yield of the reaction product are shown in Table 1. In the reaction system, the reaction between the catalyst (C1a) and the alcohol derived from the raw material (compound (3a)) causes Me (n-octyl) 3P] + [OR5]-as a catalytically active species.(Most R5 is 3-hydroxy-3-methylbutyl).

According to the analysis of related databases, 2568-33-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Nagoya University; Ishihara, Kazuaki; Hatano, Manabu; (20 pag.)JP2019/26618; (2019); A;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Adding a certain compound to certain chemical reactions, such as: 2568-33-4, 3-Methylbutane-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, 2568-33-4, blongs to alcohols-buliding-blocks compound. Computed Properties of C5H12O2

Example 123(3R*,4R*)-N-[3,5-bis(trifluoromethyl)benzyl]-3-(4-fluoro-2-methylphenyl)-1-(3-hydroxy-3-methylbutyl)-N-methylpiperidine-4-carboxamide monohydrochloride(step 1)To a solution of 3-methyl-1,3-butanediol (1.0 g) in pyridine (10 mL) was added p-toluenesulfonyl chloride (2.26 g) at 0 C., and the mixture was stirred at room temperature for 27 hr. The reaction mixture was poured into ethyl acetate, organic layer was washed with 1N hydrochloric acid and water and dried, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (solvent gradient; 0?100% ethyl acetate/hexane) to give 3-hydroxy-3-methylbutyl 4-methylbenzenesulfonate (878 mg, 35%) as a colorless oil.1H-NMR (300 MHz, CDCl3):delta 1.22 (6H, s), 1.34 (1H, s), 1.86 (2H, t, J=6.8 Hz), 2.45 (3H, s), 4.21 (2H, t, J=6.8 Hz), 7.35 (2H, d, J=8.0 Hz), 7.80 (2H, d, J=8.3 Hz)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,2568-33-4, its application will become more common.

Reference:
Patent; Shirai, Junya; Morimoto, Shinji; Sugiyama, Hideyuki; Sakauchi, Nobuki; Yoshikawa, Takeshi; US2008/275085; (2008); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts