Category: 2568-33-4

Application 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.

To a stirred solution of allene 14 (101 mg, 0.288 mmol), DMF (0.3 mL) and 3-methyl-1,3-butanediol 28 (0.16 mL, 1.47 mmol) at 0 C were added (IPr)AuCl (18.0 mg, 0.030 mmol), AgOTf (8.0 mg, 0.031 mmol) and NIS (71.0 mg, 0.316 mmol). The reaction mixture was stirred for 22 h at 0 C, after which the mixture was diluted with Et2O, filtered through a plug of silica, washed with water and brine and dried (MgSO4). The product was isolated using flash column chromatography (2:1 hexane/diethyl ether) as a colourless oil (82.3 mg, 0.142 mmol, 49%). Stereochemistry of alkene was confirmed through NOE. Rf=0.38 (1:2 hexane/diethyl ether). numax/cm-1 3454 br (OH), 1631 w (CC), 1590 w, 1472 m, 1427 m (Ar CC), 1111 s (Si-O), 1088 s (C-O); 1H NMR (200 MHz, CDCl3) delta 7.49 (10H, m, Ar-H), 5.89 (1H, t, J 6.4, CH), 3.76 (2H, t, J 6.3, SiOCH2), 3.44 (2H, t, J 5.9, OCH2), 2.49 (2H, td, J 6.3, 6.4, CH2CHC), 1.75 (2H, t, J 5.9, OCH2CH2CMe2OH), 1.44 (6H, s, CH3), 1.25 (6H, s, CH3), 1.05 (9H, s, CH3). 13C NMR (50 MHz, CDCl3) delta 135.5 (CH), 133.7 (C), 133.6 (CH), 129.7 (CH), 127.7 (CH), 120.7 (C), 78.6 (C), 70.6 (C), 62.2 (CH2), 59.9 (CH2), 41.6 (CH2), 40.5 (CH2), 29.4 (CH3), 26.9 (CH3), 26.8 (CH3), 19.2 (C). [M+NH4]+=598.2202 (calcd for C28H41IO3Si+NH4+=598.2208).

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:
Article; Heuer-Jungemann, Amelie; McLaren, Ross G.; Hadfield, Maximillian S.; Lee, Ai-Lan; Tetrahedron; vol. 67; 9; (2011); p. 1609 – 1616;,
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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, COA of Formula: C5H12O2, blongs to alcohols-buliding-blocks compound. COA of Formula: C5H12O2

To a solution of 3-methylbutane-1 ,3-diol (2.5 ml_) in dichloromethane (30 ml_) and pyridine (2.1 ml_) is added at 0C 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 HCI solution and brine. After drying (MgSO4) the solvent is evaporated and the product is pu rified by ch romatog raphy on s il ica 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]+.

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; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; ECKHARDT, Matthias; FRATTINI, Sara; HAMPRECHT, Dieter; HIMMELSBACH, Frank; LANGKOPF, Elke; LINGARD, Iain; PETERS, Stefan; WAGNER, Holger; WO2013/144097; (2013); A1;,
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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. 2568-33-4, name is 3-Methylbutane-1,3-diol. This compound has unique chemical properties. The synthetic route is as follows. category: alcohols-buliding-blocks

(210a) 3-Hydroxy-3-methylbutanal Pyridinium chlorochromate (2.6 g, 12 mmol) and Celite (5 g) were sufficiently ground in a mortar and were suspended in methylene chloride (50 mL). To this mixture, a methylene chloride solution (10 mL) of 3-methyl-1,3-butanediol (1.1 g, 10 mmol) was added. The resulting mixture was stirred at room temperature for 3 hr and then filtered. The filtrate was concentrated under reduced pressure. The resulting crude product was purified by silica gel column chromatography (Biotage, eluding solvent; hexane: ethyl acetate = 2: 3) to obtain 0.47 g (yield: 45%) of the title compound as a colorless oily material. 1H-NMR (400 MHz, CDCl3) delta ppm: 9.85 (1H, t, J = 2.0 Hz), 2.63 (2H, d, J = 2.0 Hz), 1.34 (6H, s).

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

Reference:
Patent; Sankyo Company, Limited; EP1798229; (2007); A1;,
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Application 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.

To a cooled solution of 53 (2.0 g, 19.20 mmol, 1.0eq) in dichioromethane (40 mE) was added pyridine (3.03 g,38.4 mmol, 2.0 eq) followed by mesyl chloride (2.29 g,20.16 mmol, 1.05 eq) dropwise at 0 C. The reaction mixturewas stirred at room temperature for 1 h. After completion ofreaction, reaction mixture was transferred into ice cold waterand product was extracted with dichloro methane. Organic layer was combined, dried over sodium sulphate and concentrated under reduced pressure to obtain 53.1. (1.5 g, 42.86%), MS(ES): mlz 183.06 [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 2568-33-4, 3-Methylbutane-1,3-diol.

Reference:
Patent; Nimbus Lakshmi, Inc.; Masse, Craig E.; Greenwood, Jeremy Robert; Mondal, Sayan; Cowen, Scott D.; McLean, Thomas H.; (624 pag.)US2019/31664; (2019); 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. 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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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, SDS of cas: 2568-33-4, blongs to alcohols-buliding-blocks compound. SDS of cas: 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).

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; Nagoya University; Ishihara, Kazuaki; Hatano, Manabu; (20 pag.)JP2019/26618; (2019); A;,
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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, Safety of 3-Methylbutane-1,3-diol, blongs to alcohols-buliding-blocks compound. Safety of 3-Methylbutane-1,3-diol

To a solution of ethyl (2E) -3- (2-{ [3-chloro-5- (trifluoromethyl)pyridin-2-yl]oxy}-4-hydroxyphenyl) acrylate (10.0 g) in tetrahydrofuran (300 ml) were added tributylphosphine (10.5 ml), 3-methylbutane-l, 3-diol (4.0 ml) and 1, 1′ – (azodicarbonyl) dipiperidine (9.7,6 g) , and the mixture was stirred overnight at 500C. Then, tributylphosphine (10.5 ml), 3-methylbutane-l, 3-diol (4.0 ml) and 1,1′- (azodicarbonyl) dipiperidine (9.76 g) were added, and the mixture was stirred at 500C for 1 hr. The reaction mixture was concentrated, the obtained solid was washed with diisopropyl ether, and the filtrate was concentrated. The obtained residue was subjected to basic silica gel column chromatography, and eluted with ethyl acetate-hexane (hexane alone to 45:55, v/v). The obtained residue was subjected to silica gel column chromatography, and eluted with ethyl acetate-hexane (hexane alone to 3:7, v/v) to give ethyl (2E) -3- [2-{ [3-chloro-5- (trifluoromethyl)pyridin-2-yl]oxy}-4- (3-hydroxy-3- methylbutoxy) phenyl] acrylate (Reference Example 264) (1.46. g, yield: 12-%) ,as a pale-yellow solid. Recrystallization from ethyl acetate-hexane gave white crystals as 0.5 hydrate, melting point 63.5-66.00C.Then, ethyl (2E) -3- [2-{ [3-chloro-5-(trifluoromethyl) pyridin-2-yl] oxy}-4- (3-hydroxy-l, 1- dimethylpropoxy) phenyl] acrylate (Reference Example 265) (0.71 g, yield: 6%) was obtained as an orange oil.1H-NMR (300 MHz, DMSO-ds)delta: 1.20 (3 H, t, J = 7,2 Hz), 1.32 (6 H, s), 1.87 (2 H, t, J = 7.5 Hz), 3.55 – 3.62 (2 H, m) , 4.12 (2 H, q, J = 7.2 Hz), 4.40 (1 H, t, J = 5.4 Hz), 6.57 (1 H, d, J = 16.2 Hz), 6.96 (1 H, s) , 6.94 – 6.99 (1 H, m) , 7.55 (1 H, d, J = 16.2 Hz), 8.50 – 8.50 (1 H, m) , 8.63 (1 H, d, J = 2.0 EPO Hz ) .

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; TAKEDA PHARMACEUTICAL COMPANY LIMITED; WO2007/18314; (2007); A2;,
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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. 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. Quality Control of 3-Methylbutane-1,3-diol

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 × 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, 5.1 g of Zn-acetylacetonate and 33 g of hexane as a catalyst, and the inside of the system was heated to 100 to 110 C. with stirring. 15 g of hexane was withdrawn from the top of the distillation column.After cooling the inside of the system to 40 C., 240 g of methyl methacrylate and 0.24 g of 2,2,6,6-tetramethyl-4-hydroxypiperidine-N-oxide as a polymerization inhibitor were charged and stirred while blowing in a small amount of air While heating the inside of the system to 100 to 130 C. Methanol produced as the reaction proceeds proceeds by azeotropic distillation with methyl methacrylate,The reaction was gradually withdrawn from the top of the distillation column to proceed the reaction.The conversion rate of 3-methyl-3-hydroxy-1-butyl alcohol after 7 hours from the start of the reaction was 97.5%3-methyl-3-hydroxy-1-butyl alcoholThe yield of 3-methyl-3-hydroxy-1-butyl methacrylate was 77.0%, and the diester yield based on 3-methyl-3-hydroxy-1-butyl alcohol was 10.8%

With the rapid development of chemical substances, we look forward to future research findings about 2568-33-4.

Reference:
Patent; Mitsubishi Gas Chemical Company; Kushida, Eriko; Takemoto, Makiko; (16 pag.)JP2018/135285; (2018); A;,
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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.

General procedure: 5-bromo-2-chloropyrimidine (1.0 equiv.) was solvated in DMF (0.2 M) along with the appropriate diol (2.0 equiv.). 60% sodium hydride in mineral oil (3.0 equiv.) was added to the reaction mixture portion-wise at 0 C, then the reaction mixtureallowed to warm to room temperature and stirred for 30 minutes. The reaction mixture was then quenched with saturated ammonium chloride and diluted with EtOAc. The organic layer was washed with 10% aqueous LiC1 solution (3x), brine (lx), dried with sodium sulfate, filtered and concentrated. The resulting residue was dissolved in methylene chloride before being purified by silica gel chromatography to provide thedesired material.; This intermediate was prepared according to Procedure A from3-methylbutane-1,3-diol. Intermediate I-bOA was afforded in 68% yield after silica gel chromatography. LC-MS: Method H, MS (ESI) m/z: 263.0. ?H NMR (400MHz, CDC13)8.55 (s, 2H), 4.56 (t, J=6.8 Hz, 2H), 2.05 (t, J=6.8 Hz, 2H), 1.34 (s, 6H).

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; BRISTOL-MYERS SQUIBB COMPANY; ZHANG, Xiaojun; PRIESTLEY, Eldon Scott; BATES, J. Alex; HALPERN, Oz Scott; REZNIK, Samuel Kaye; RICHTER, Jeremy M.; (1137 pag.)WO2018/13774; (2018); A1;,
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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.

EXAMPLE 84-(4-Fluorobenzyloxy)- 1-[4-(3 -hydroxy-3 -methylbutoxy)-3 -methoxyphenyl]pyridin-2-( lH)-oneTo a solution of 4-[(4-fluorobenzyloxy)-l-(4-hydroxy-3-methoxyphenyl) pyridin-2(lH)- one (25 mg, 0.073 mmol), 3-methylbutane-l, 3-diol (11 mg, 0.11 mmol) and triphenylphosphine (19 mg, 0.073 mmol) in anhydrous THF (0.5 mL) under N2 atmosphere at 0C, diisopropyl azodicarboxylate (14 mg, 0.080 mmol) was added. After stirring at rt overnight, the volatiles were removed under reduced pressure, and the residue was purified with preparative HPLC eluting with water /acetonitrile (containing 0.1%TFA, 37 % to 67 %) to afford the title compound. 1HNMR (400MHz, CDC13, delta ppm): 7.39-7.53 (3H, m), 7.12 (2H, t, J= 8.8Hz), 7.04-7.09 (IH, m), 6.88-6.97 (IH, m), 6.78-6.86 (IH, m), 6.20-6.28 (IH, m), 6.05-6.09 (IH, m), 5.12 (2H, s), 4.12- 4.21 (2H, m), 3.84 (3H, s), 1.99 (2H, t, J= 6.8 Hz), 1.26 (6H, s). LCMS: m/e 428 [M+H]+.

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; MERCK SHARP & DOHME CORP.; LIN, Linus; SOLL, Richard; DONG, Jingchao; WU, Hao; SUZUKI, Takao; HU, Bin; LIU, Dejun; HAO, Jinglai; XU, Ming; WO2011/127643; (2011); A1;,
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