Category: 96-35-5

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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Adding a certain compound to certain chemical reactions, such as: 96-35-5, Methyl 2-hydroxyacetate, 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, Product Details of 96-35-5, blongs to alcohols-buliding-blocks compound. Product Details of 96-35-5

4-(3-(3-Fluoro-4-hydroxyphenyl)-4,4-dimethyl-5-oxo-2-thioxoimidazolidin-1-yl)-2-(trifluoromethyl)benzonitrile 1e (100 mg, 0.24 mmol) was placed in a reaction flask, followed by addition of methyl glycolate (42 mg, 0.47 mmol), triphenylphosphine (93 mg, 0.35 mmol), 5 mL of dichloromethane, and diisopropyl azodicarboxylate (72 mg, 0.35 mmol), successively. The reaction solution was stirred for 1 hour. The reaction solution was concentrated under reduced pressure, and the residue was purified by thin layer chromatography with elution system A to obtain the title compound methyl 2-(4-(3-(4-cyano-3-(trifluoromethyl)phenyl)-5,5-dimethyl-4-oxo-2-thioxoimidazolidin-1-yl)-2-fluorophenoxy)acetate 31a (104 mg, yield 89.7%) as a white solid. MS m/z (ESI): 496.2 [M+1]

At the same time, in my other blogs, there are other synthetic methods of this type of compound,96-35-5, Methyl 2-hydroxyacetate, and friends who are interested can also refer to it.

Reference:
Patent; Shanghai Hengrui Pharmaceutical Co., Ltd.; Jiangsu Hengrui Medicine Co., Ltd.; Lu, Hejun; Sun, Piaoyang; Fei, Hongbo; Jiang, Hongjian; Wang, Haowei; Dong, Qing; US2015/225381; (2015); 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.96-35-5, name is Methyl 2-hydroxyacetate, molecular formula is C3H6O3, molecular weight is 90.08, as common compound, the synthetic route is as follows.SDS of cas: 96-35-5

Intermediate 4: 4-oxotetrahydrofuran-3-carbonitrile [00211] To a solution of potassium tert-butoxide (24.91g, 222.O3mmol) in THF (200mL) at 0Cwas added methyl glycolate (20.OOmL, 259mmo1) dropwise. The mixture was left to stir for 10 minutes before adding acrylonitrile (14.62mL, 222mmo1) dropwise. The reaction then allowed to warm to room temperature and left to stir for 3 hours. Water and EtOAc were added to the reaction mixture and the layers separated. The aqueous layer as then acidified to pHi with 1 M HCI and extracted twice with EtOAc. The combined organic layers were then washed with brine, dried over Na2SO4 and then passed through a hydrophobic frit before being concentrated under reducedpressure to afford 4-oxotetrahydrofuran-3-carbonitrile (10.29g, 93mmol, 42% yield) as a yellow solid.1H NMR (CDCI3, 400MHz) O/ppm: 4.65 (1H, t, J= 9.3Hz), 4.26 (1H, t, J= 9.3Hz), 4.18 (1H, d, J=17.5Hz), 4.02 (1H, d, J= 17.5Hz), 3.61 (1H, t, J= 9.3Hz).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,96-35-5, Methyl 2-hydroxyacetate, and friends who are interested can also refer to it.

Reference:
Patent; REDX PHARMA PLC; ARMER, Richard; BELFIELD, Andrew; BINGHAM, Matilda; JOHNSON, Alice; MARGATHE, Jean-Francois; AVERY, Craig; HUGHES, Shaun; MORRISON, Angus; (278 pag.)WO2016/51193; (2016); A1;,
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Electric Literature of 96-35-5 ,Some common heterocyclic compound, 96-35-5, molecular formula is C3H6O3, 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.

As a reactive distillation apparatus, an apparatus obtained by connecting a 3-stage packed column to a flask and further providing a refluxing device at the top of the packed column was used. A mixed liquid obtained by mixing 150 g of water with 50 g of the distillate containing more than 98 wt % of methyl glycolate obtained in (3) above was put into the flask. Next, reactive distillation was carried out for 2 hours at normal pressure, maintaining the temperature at the base of the column of the reactive distillation apparatus (i.e. the liquid temperature) at 95 to 97 C. At this time, distillate containing methanol was distilled off. The temperature at the top of the column was 65 C. at the start of the reactive distillation, but had reached 100 C. by the end. [0322] After the reactive distillation had been completed, 114 g of an aqueous solution containing 36.1 wt % of glycolic acid was recovered from the flask. The yield of glycolic acid relative to the methyl glycolate was 100%. Regarding impurities, formaldehyde and chlorine compounds were not detected, and 20 ppm of oxalic acid and 76 ppm of ethylene glycol were detected.

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. 96-35-5, Methyl 2-hydroxyacetate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Hayashi, Toshio; Baba, Hideyuki; US2004/138409; (2004); A1;,
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Synthetic Route of 96-35-5 ,Some common heterocyclic compound, 96-35-5, molecular formula is C3H6O3, 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.

3.85 g of silver perchlorate (18.6 mmol) are added to a solution of 8,8-dibromobicyclo[5.1.0]octane 16 (2.5 g, 9.3 mmol) and methyl glycolate (6.35 ml, 83.9 mmol) dissolved in 5 ml of anhydrous toluene in a dry round-bottomed flask under Ar protected from light by an aluminum film. The reaction mixture is stirred at ambient temperature for 1 h 30 and then the silver salts are filtered off through a sintered glass funnel and washed with AcOEt. The solution is concentrated under vacuum to give a viscous brown oil which is purified by chromatography on silica gel (cyclohexane/2-15% AcOEt) to produce 17 in the form of a yellow oil (w=1.7 g, i.e. 66% yield).1H NMR (CDCl3, 200 MHz): delta (ppm) 0.7-2.2 (m, 8H, H4-4′-5-5′-6-6′-7-7′); 2.28 (m, 1H, H8); 2.70 (ddd, J=5.0-11.5-23.5 Hz, 1H, H8′); 3.72 (s, 3H, OMe); 3.94 (d, J=16.5 Hz, 1H, H9); 4.10 (dd, J=5.0-10.0 Hz, 1H, H3); 4.23 (d, J=16.5 Hz, 1H, H9′); 6.20 (dd, J=4.0-11.5 Hz, 1H, H1).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,96-35-5, its application will become more common.

Reference:
Patent; COMMISSARIAT A L’ENERGIE ATOMIQUE ET AUX ENERGIES ALTERNATIVES; US2011/118484; (2011); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Reference of 96-35-5 ,Some common heterocyclic compound, 96-35-5, molecular formula is C3H6O3, 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.

Intermediate P1082-phenyl-4,6-dihydro-2H-furo [3 ,4-c]pyrazol-31006951 Step A: Preparation of 4-oxotetrahydrofuran-3-carbonitrile: To a suspension of KOtBu (996.6 mg, 8.88 1 mmol) in THF (640.4 mg, 8.88 1 mmol) cooled to 0 C was added dropwise methyl 2-hydroxyacetate (675.7 jiL, 8.881 mmol) and stirred for 10 minutes. The acrylonitrile (589.1 jiL, 8.881 mmol) was then added and the reaction stirred at ambient temperature. After 3 hours, the reaction was diluted with 1120 (50 mL), then extracted with Et20 (25 mL) to remove any starting ester. The basic aqueous phase was acidified with 2M HC1 (5 mL), then extracted with Et20 (2 x 50 mL). The combined organic phases were dried with MgSO4, filtered, and concentrated to afford a light brown oil (446 mg, 45.2% yield). ?H NMR (CDC13) 4.63 (t, 111), 4.24 (t, 111), 4.14 (d, 1H), 4.02 (d, 1H), 3.57 (t, 111).

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. 96-35-5, Methyl 2-hydroxyacetate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ARRAY BIOPHARMA INC.; BLAKE, James F.; BRANDHUBER, Barbara J.; HAAS, Julia; NEWHOUSE, Brad; THOMAS, Allen A.; WINSKI, Shannon L.; WO2014/78331; (2014); 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.

Preparation 69: 2-Hydroxyacetohydrazide Hydrazine monohydrate (1.08 g, 22.2 mmol) was added to a solution of methyl glycolate (0.84 mL, 11.1 mmol) in methanol (10 mL) and the mixture was heated under reflux for 2 hours and stirred at room temperature for 72 hours. The reaction mixture was then concentrated in vacuo to afford the title compound as a white solid in quantitative yield. 1H NMR(400 MHz, CDCl3) delta: 4.04(s, 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 96-35-5, Methyl 2-hydroxyacetate.

Reference:
Patent; Pfizer Inc; US2006/160786; (2006); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Adding a certain compound to certain chemical reactions, such as: 96-35-5, Methyl 2-hydroxyacetate, 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 Methyl 2-hydroxyacetate, blongs to alcohols-buliding-blocks compound. Safety of Methyl 2-hydroxyacetate

To 17.09 g of Compound (5) shown below (methyl glycolate, manufactured by TCI), 30,00 g of tetrahydrofuran (THF) was added, and 21.15 g of triethylamine was further added. The mixture was cooled to 0C, and 20.85 g of methacrylic acid chloride was then added dropwise. After returning the temperature to room temperature, the mixture was stirred for 2 hours. A sodium hydrogencarbonate aqueous solution was added, followed by extraction with ethyl acetate. Organic layers were gathered, to which was then added MgSO4, and the resulting mixture was filtered and concentrated to obtain 28.51 g of Compound (6) (yield: 95 %). 1H-NMR, (400 MHz in (CD3)2CO): ? (ppm) = 1.94 to 2.04 (3H), 3.71 to 3.72 (3H), 4.73 (2H), 5.72 (1H), 6.15 (1H)

The synthetic route of 96-35-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Fujifilm Corporation; EP2196462; (2010); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Reference of 96-35-5, 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 96-35-5 as follows.

To a suspension of KOtBu (996.6 mg, 8.881 mmol) in THF (640.4 mg, 8.881 mmol) cooled to 0 C was added dropwise methyl 2-hydroxyacetate (675.7 mu, 8.881 mmol) and stirred for 10 minutes. The acrylonitrile (589.1 mu, 8.881 mmol) was then added and the reaction stirred at ambient temperature. After 3 hours, the reaction was diluted with H20 (50 mL), then extracted with Et20 (25 mL) to remove any starting ester. The basic aqueous phase was acidified with 2M HCl (5 mL), then extracted with Et20 (2 x 50 mL). The combined organic phases were dried with MgS04, filtered, and concentrated to afford a light brown oil (446 mg, 45.2% yield). FontWeight=”Bold” FontSize=”10″ H NMR (CDC13) delta 4.63 (t, 1H), 4.24 (t, 1H), 4.14 (d, 1H), 4.02 (d, 1H), 3.57 (t, 1H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,96-35-5, its application will become more common.

Reference:
Patent; ARRAY BIOPHARMA INC.; ALLEN, Shelley; ANDREWS, Steven, Wade; BLAKE, James, F.; BRANDHUBER, Barbara, J.; HAAS, Julia; JIANG, Yutong; KERCHER, Timothy; KOLAKOWSKI, Gabrielle, R.; THOMAS, Allen, A.; WINSKI, Shannon, L.; WO2014/78454; (2014); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

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. name: Methyl 2-hydroxyacetate

A certain amount of methacryloyl chloride (0.144 mol) dissolved in anhydrous DCM (60 mL) was added dropwise to methyl glycolate (at a temperature of ?0 C and an argon (Ar) atmosphere) 0.144 mol), TEA (0.288 mol), anhydrous DCM (100 mL), stir overnight, wash and purify, and obtain pure product by column chromatography.

With the rapid development of chemical substances, we look forward to future research findings about 96-35-5.

Reference:
Patent; Southwest University; Xu Zhigang; Shi Xiaoxiao; Ma Xiaoqian; Bai Shuang; Xue Peng; Kang Yuejun; (15 pag.)CN107596383; (2019); B;,
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Alcohols – Chemistry LibreTexts