Tag: M.W=0-100

Related Products of 110-73-6, 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. 110-73-6, name is 2-(Ethylamino)ethanol. A new synthetic method of this compound is introduced below.

In a 100 mL 1-neck round bottom flask [A-1] (Benzenesulfonate Dichlorosulfofluorescein) (3g, 7.40mmol, 1eq), [A-2] (2-(Ethylamino)ethanol) (5.28g, 59.22mmol, 8eq), After adding 50 g of di-water, the mixture was stirred at 100C. Thereafter, the reaction was performed overnight (overnight, 12 hours). The reaction was terminated by quenching in 1M HCl solution, NaCl (sodium chloride) was added to precipitate the reaction. The resulting precipitate was filtered under reduced pressure and dried in an oven at 80C. DMF (Dimethylformamide) to remove NaCl between products after drying After dissolving in filtration, the filtrate was diethyl ether Quenching on The mixture was filtered under reduced pressure and dried to obtain Compound A (2.88 g, 5.64 mmol, 76%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,110-73-6, 2-(Ethylamino)ethanol, and friends who are interested can also refer to it.

Reference:
Patent; LG Chem, Ltd.; Choi Sang-a; Lee Da-mi; Yang Seung-jin; Lee Jae-yong; Kim Hye-jin; Kim Yeong-ung; (47 pag.)KR2020/46212; (2020); A;,
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Related Products 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.

A mixture ofmethyl 2-hydroxyacetate (9 g, 0.1 mol,equiv) and hydrazine hydrate (9.6 ml, 1.5 equiv, 85%) in methanol (100 ml) was refluxed for 8 h before methanol and exceesive hydrazine hydrate were evaporated. Toluene was added and evaporated again to remove the residual water to give the title compound as a white solid which could be used in next step without further purification.

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; Shen, Jianhua; Wang, Yiping; Wang, Kai; US2014/171431; (2014); A1;,
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Synthetic Route of 33420-52-9, Adding some certain compound to certain chemical reactions, such as: 33420-52-9, name is 2,2-Difluoropropan-1-ol,molecular formula is C3H6F2O, 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 33420-52-9.

To a cooled (0 C) solution of 2,2-difluoropropan-l-ol (3.17 g, 33.0 mmol) and pyridine (2.97 mL, 36.7 mmol) in CH3CN (100 mL) was added dropwise Tf20 (5.70 mL, 33.8 mmol). The reaction was stirred for 30 min at 0 C. To the cooled slurry was added a cold solution of methyl 4-methyl-5-(l-(piperidin-4-yl)propyl)thiophene-3 -carboxylate hydrochloride (2.6 g, 7.34 mmol) and K2C03 (9.13 g, 66.0 mmol) in CH3CN (20 mL). The reaction was allowed to warm to RT, then heated at 50 C overnight. The reaction was evaporated to dryness under vacuum, taken up in DCM, washed with water, brine, dried (Na2S04), filtered, and concentrated under vacuum. The residue was purified by silica gel chromatography (Isco RediSep Rf Gold 120 g, 5% EtOAc:hexanes) to give methyl 5-(1- (1-(2,2-difluoropropyl)piperidin-4-yl)propyl)-4-methylthiophene-3-carboxylate (2.05 g, 5.42 mmol, 73.8 % yield) as a yellow oil. 1H NMR (400 MHz, CDCl3) delta 8.00 (s, 1H), 3.85 (s, 3H), 2.99 (d, J=11.12 Hz, 1H), 2.86 (d, J=11.12 Hz, 1H), 2.53-2.75 (m, 3H), 2.37 (s, 3H), 2.04-2.27 (m, 2H), 1.84-2.01 (m, 2H), 1.62 (t, J=18.69 Hz, 4H), 1.30-1.47 (m, 5H), 0.76 (t, J=7.33 Hz, 3H). MS(ES) [M+H]+ 360.2.

According to the analysis of related databases, 33420-52-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY (NO.2) LIMITED; KNIGHT, Steven David; NEWLANDER, Kenneth Allen; TIAN, Xinrong; (112 pag.)WO2016/66697; (2016); A1;,
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Electric Literature of 96-35-5, 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. 96-35-5, name is Methyl 2-hydroxyacetate, molecular formula is C3H6O3, 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: Hydrogenation of Other Ester Compounds Catalyzed by Synthetic Preparation of Bipyridine Tetradshed Ruthenium Complex 5 The results are shown in Table 2:Table 2 Hydrogenation of other ester compounds a; A Reaction conditions: S / C = 1000,3.0 mmol Substrate, 3.0 mumol 5, 3.0 mL lPrOH, 0.3 mmol NaOMe, 5 MPa H2, 25 C; D 100 C.

According to the analysis of related databases, 96-35-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Nankai University; Zhou, Qilin; Li, Wei; Xie, Jianhua; Wang, Lixin; (22 pag.)CN103980317; (2017); B;,
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Adding a certain compound to certain chemical reactions, such as: 109-83-1, 2-(Methylamino)ethanol, 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, 109-83-1, blongs to alcohols-buliding-blocks compound. Recommanded Product: 109-83-1

EXAMPLE 207 2-N-methyl-benzyloxycarbonylaminoethanol To N-methyl ethanolamine (149 mmol) in methylene chloride (100 ml) at 0 C. was added benzyl chloroformate (70 mmol). The mixture was stirred at 0 C. for 30 min, then at room temperature for 1 h, poured into ethyl acetate, washed with 2M HCl, saturated NaHCO3 solution and then brine, then dried over Na2 SO4 and evaporated to provide the desired compound. NMR (CDCl3) 3.01 (s, 3H), 3.47 (m, 2H), 3.78 (m, 2H), 5.14 (s, 2H), 7.36 (m, 5H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,109-83-1, its application will become more common.

Reference:
Patent; Abbott Laboratories; US5032577; (1991); A;,
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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.2002-24-6, name is 2-Aminoethanol hydrochloride, molecular formula is C2H8ClNO, molecular weight is 97.544, as common compound, the synthetic route is as follows.name: 2-Aminoethanol hydrochloride

A dichloromethane (5 ml) solution of the [6-[(4-chlorophenylsulfonyl)(2,5-difluorophenyl)methyl]pyridin-3-yl]carboxylic acid (100 mg, 0.236 mmol) obtained in Example 50 were added triethylamine (80 mul, 0.566 mmol), 4-dimethylaminopyridine (15 mg, 0.118 mmol), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (54 mg, 0.283 mmol) and ethanolamine hydrochloride (28 mg, 0.283 mmol). The resulting mixture was stirred at room temperature for 17.5 hours. The reaction mixture was diluted with dichloromethane. The diluted mixture was washed sequentially with water, a saturated aqueous solution of sodium bicarbonate and brine. The organic layer thus obtained was dried over magnesium sulfate and concentrated under reduced pressure. The residue thus obtained was subjected to flash silica gel column chromatography. The fraction obtained from the dichloromethane_methanol=30:1 eluate was concentrated under reduced pressure to give the title compound (69 mg, 0.148 mmol, 63%) as a white powder. 1H-NMR (400MHz, CDCl3) delta: 2.38 (1H,t, J=4.9Hz), 3.65 (2H,td, J=5.4, 4.9Hz), 3.85 (2H,q, J=4.6Hz), 5.99 (1H,s), 6.77 (1H,brs), 6.90-6.96 (1H,m), 7.00-7.06 (1H,m), 7.42 (2H,d, J=8.6Hz), 7.56 (2H,d, J=8.6Hz), 7.70 (1H,d, J=8.1Hz), 7.97-8.01 (1H,m), 8.15 (1H,dd, J=8.1, 2.2Hz), 8.99 (1H,d, J=2.2Hz)H,m), mp: 179 to 181C. Elemental Analysis for C21H17ClF2N2O4S: Calculated: C,54.02; H, 3.67; Cl, 7.59; F,8.14; N,6.00; S,6.87. Found: C, 53.83; H,3.63; Cl, 7.72; F, 8.14; N,6.06; S, 7.02.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2002-24-6, 2-Aminoethanol hydrochloride, and friends who are interested can also refer to it.

Reference:
Patent; DAIICHI PHARMACEUTICAL CO., LTD.; EP1640366; (2006); A1;,
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Reference of 96-35-5, 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. 96-35-5, name is Methyl 2-hydroxyacetate, molecular formula is C3H6O3, 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.

Example 1Reduction of Methyl Glycolate in Methanol to Ethylene Glycol The following example shows the positive effect of adding a promoter to the catalyst mixture. Run 1 in the table below is a comparative example. Runs 2-9 represent variants of the current invention.A 300-milliliter autoclave was charged with Ru(Acac)3 (0.10 mmole), TRIPHOS (0.50 mmole), and the promoter in the amount specified in the table. Methanol (32 milliliters) and methyl glycolate (0.156 mole) were added, and the reactor was sealed under N2. The reactor was pressurized to 250 psig (1.7 MPa) with H2 and heated to 200 C. Upon reaching 200 C., the H2 pressure was raised to 2000 psig (13.8 MPa). The autoclave was stirred and held at 200 C., 2000 psig (13.8 MPa) for a total of 3 hours. The autoclave was then cooled, excess gas vented, and the contents recovered. The contents were analyzed by the use of an internal standard gas chromatography method for the presence of methyl glycolate (?MG?) and ethylene glycol (?EG?). The results are shown in the table below. Catalyst Activity Rate Amount of Conversion of Selectivity to (moles EG per Promoter MG EG mole of Ru Run Promoter (mmole) (%) (%) per hr) 1 none none 39.5 88.4 205 2 Zn 0.25 49.3 88.9 228 Acetonylacetonate 3Me4NBF4 0.025 99.7 98.2 509 4Me4NBF4 0.001 96.8 98.2 394 5NH4PF6 0.025 100 96.9 504 6NH4OAc 0.150 67.8 94.8 334 7Ph4PBr 0.025 84.1 97.8 428 8NaPh4B 0.500 81.1 93.5 394 9BuN4PF6 0.025 97.8 95.8 487 Analysis of the run without a promoter showed a 39.5% conversion of the methyl glycolate with 88.4% selectivity to ethylene glycol. The catalyst activity rate for this experiment was 205 moles of EG per mole of ruthenium per hour. On the other hand, runs with a promoter showed MG conversions of 49-100%, EG selectivities of 89-98%, and catalyst activity rates of 230-510 moles of EG per mole of ruthenium per hour. This data show the positive effects of adding a promoter to the reaction mixture.

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; EASTMAN CHEMICAL COMPANY; US2009/143612; (2009); A1;,
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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.124-68-5, name is 2-Amino-2-methyl-1-propanol, molecular formula is C4H11NO, molecular weight is 89.1362, as common compound, the synthetic route is as follows.HPLC of Formula: C4H11NO

Example 24d 2-amino-6-(2-amino-2-methylpropoxy)benzonitrile To a solution of 2-amino-2-methylpropan-1-ol (14.4 g, 161 mmol) in anhydrous THF (150 mL) was added NaH (6.8 g, 161 mmol, 60% in mineral oil) in small portions at 0 C. under nitrogen. The mixture was stirred at 0 C. for 30 minutes and then stirred at room temperature for another 30 minutes. The solution was cooled down to 0 C. again, and to this solution was added dropwise a solution of 2-amino-6-fluorobenzonitrile (20.0 g, 147 mmol) in anhydrous THF (50 mL). The reaction mixture was then refluxed overnight under nitrogen. The reaction mixture was cooled down to room temperature and carefully quenched with aqueous NH4Cl solution and extracted with ethyl acetate (3*). The combined organic layers were washed with brine, dried over MgSO4, filtered and concentrated. The crude mixture was purified by chromatography on silica gel eluting with 10% MeOH in DCM to give the title compound as yellow solid (23.4 g 71%). 1H NMR (400 MHz, DMSO-d6) delta 1.08 (s, 6H), 3.15 (s, 2H), 3.64 (s, 2H), 5.98 (s, 2H), 6.13 (d, J=8.0 Hz, 1H), 6.31 (d, J=8.4 Hz, 1H), 7.15 (t, J=8.4 Hz, 1H). MS 236 (MH+).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,124-68-5, 2-Amino-2-methyl-1-propanol, and friends who are interested can also refer to it.

Reference:
Patent; SENOMYX, INC.; US2012/41078; (2012); A1;,
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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.2919-23-5, name is Cyclobutanol, molecular formula is C4H8O, molecular weight is 72.1057, as common compound, the synthetic route is as follows.Computed Properties of C4H8O

a) 5-Bromo-6-cyclobutoxy-3-pyridinecarboxylic acid 5-Bromo-6-chloro-3-pyridinecarboxylic acid (CAN 29241-62-1, 2.0 g, 8.46 mmol) was dissolved in DMSO (20.0 mL). Cyclobutanol (793 mg, 857 ??, 11.0 mmol) and potassium hydroxide powder (1.42 g, 25.4 mmol) were added and the mixture was stirred at room temperature overnight. Water (20 mL) was added and the mixture was acidified (under ice-water bath cooling) with 37% HC1 in water (pH = 2). The suspension was filtered, washed with water and the solid was dried to yield 1.88 g (82%) of the title compound as a white solid; MS (ESI): 270.2 (M-H)~. b) 5-(4-Chloro-phenyl)-6-cyclobutoxy-3-pyridinecarboxylic acid

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2919-23-5, Cyclobutanol, and friends who are interested can also refer to it.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; GRETHER, Uwe; HEBEISEN, Paul; MOHR, Peter; RICKLIN, Fabienne; ROEVER, Stephan; WO2013/37703; (2013); A1;,
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Related Products of 2854-16-2, 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 2854-16-2 as follows.

Example 19N-(2-{[(2-hydroxy-2-methylpropyl)amino]methyl}-1-methyl-1H-indol-5-yl}-4-[(2S)-tetrahydrofuran-2-ylmethoxy]benzamideN-(2-Formyl-1-methyl-1H-indol-5-yl)-4-[(2S)-tetrahydrofuran-2-ylmethoxy]benzamide (300 mg) obtained in Reference Example 10 and 1-amino-2-methylpropan-2-ol (143 mg) were suspended in NMP (3.0 mL), acetic acid (1.0 mL) was added at room temperature, and the mixture was stirred at the same temperature for 3 hr.Sodium triacetoxyborohydride (336 mg) was added, the mixture was stirred at room temperature for 90 hr, and diluted with ethyl acetate, and 2N aqueous sodium hydroxide solution (20 mL) was added at room temperature.The mixture was poured into THF-water, and the organic layer was washed twice with saturated brine, dried over sodium sulfate, and concentrated under reduced pressure.The obtained solid was suspended in ethyl acetate, and the precipitate was collected by filtration, washed with ethyl acetate, and dried under reduced pressure to give the title compound (323 mg, yield 90percent) as a pale-brown solid.1H NMR (300 MHz, CDCl3) delta: 1.19 (6 H, s), 1.71 – 1.88 (1 H, m), 1.90 – 2.20 (3 H, m), 2.65 (2 H, s), 2.77 (1 H, br. s.), 3.78 (3 H, s), 3.80 – 3.90 (1 H, m), 3.90 – 4.01 (3 H, m), 4.04 (2 H, d, J=4.9 Hz), 4.31 (1 H, tt, J=7.0, 5.3 Hz), 6.38 (1 H, s), 7.01 (2 H, d, J=8.7 Hz), 7.24 – 7.29 (1 H, m), 7.30 – 7.36 (1 H, m), 7.75 (1 H, s), 7.86 (2 H, d, J=9.1 Hz), 7.88 (1 H, s).melting point: 188-190°Celemental analysis (C26H33N3O4)Calculated: C, 69.16; H, 7.37; N, 9.31.Found: C, 69.02; H, 7.47; N, 9.30.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,2854-16-2, its application will become more common.

Reference:
Patent; Takeda Pharmaceutical Company Limited; EP2522657; (2012); A1;,
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