Category: alcohols-buliding-blocks

Adding a certain compound to certain chemical reactions, such as: 2807-30-9, 2-Propoxyethanol, 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, Recommanded Product: 2-Propoxyethanol, blongs to alcohols-buliding-blocks compound. Recommanded Product: 2-Propoxyethanol

example: of pretilachlor, wherein the steps of specific reaction of producing pretilachlor is: Reacting the ethylene glycol monopropyl The present invention comprises a process for the production ether with thionyl chloride to form a chloroether, carried out condensation reaction of chloroether with aniline to obtain a condensation product. The condensed product is distillated to obtain distilled amine ether, and the distilled amine ether is subjected to an acylation reaction to obtain pretilachlor. In the step of producing the chloroether, the thionyl chloride is mixed with the ethylene glycol monopropyl ether by dropwise addition.The step of producing the chlorinated ether is: The ethylene glycol monopropyl ether placed into the reactor, stirring, thionyl chloride was added drop wise. after the completion of drop wise addition the insulation reaction was carried out for 2 hours to produce hydrogen chloride and sulfur dioxide tail gas and chloroether. the mentioned produced chloroether further comprises the step of treating the hydrogen chloride and the sulfur dioxide tail gas, wherein the step of treating the hydrogen chloride and the sulfur dioxide tail gas is: Hydrogen chloride and sulfur dioxide tail gas are absorbed by both water and alkali, hydrogen chloride prepared hydrochloric acid and sulfur dioxide made of sodium sulfite.The step of carrying out the condensation reaction of the chloroether with aniline is: Aniline and chloroether placed into the reactor, raise the reaction temperature using thermal conductive oil , the end of the reaction layers were separated by adding liquid caustic, oil layer into the next distillation step, water layer was drained. The step of distillating the condensed product to obtain a rectified amine ether is: The condensation product is added to the aniline distillation kettle and carried out distillation, an excess of aniline is separated and applied, then amine ether was placed into distillation kettle to carried distillation of amine ether until the acceptance of qualified amine ether and a small amount of high boiling point residue was directly slag discharged.the steps of acylation reaction of distilled amine ether is as follow: after the qualified amine ether was metered it was put into the acylation kettle, and then placed into the solvent of toluene and liquid caustic soda, slowly dropwise added the measured Chloroacetyl chloride and after the completion of the dropwise addition the reaction was incubation for one hour. then it was placed into the water kettle and wash with water. The upper layer into the desolvation process and the water layer to the sewage treatment. the steps of mentioned desolvation process is: the washed pretilachlor and toluene liquid put into the lifting film for desolvation and the solvent into the application appliquer and finally obtained pretilachlor crude oil .

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2807-30-9, 2-Propoxyethanol, and friends who are interested can also refer to it.

Reference:
Patent; Jiangsu Huifeng Technology Co Ltd; Sun, Lei; He, erjin; Mao, Jian; Zhu, Jianmin; Xu, Xujin; Zhao, Jianlong; Zhang, DaLiang; Tian, tongmei; (4 pag.)CN105272869; (2016); 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.67853-03-6, name is Methyl 3-(hydroxymethyl)benzoate, molecular formula is C9H10O3, molecular weight is 166.1739, as common compound, the synthetic route is as follows.Computed Properties of C9H10O3

To a solution of PI-23a (4.1 g, 24.7 mmol, 1.0 eq) in THF (100 mL) was successively added 1,4-hydroquinone (5.4 g, 49.4 mmol, 2.0 eq), PPh3 (13.0 g, 49.4 mmol, 2.0 eq) and DEAD (8.6 g, 49.4 mmol, 2.0 eq) at 0C. The mixture was allowed to warm to room temperature and stirred for 16 h. Then the mixture was quenched with H2O (100 mL) and extracted with ethyl acetate (2100 mL). The combined organic layers were dried over anhydrous Na2SO4 and concentrated under reduced pressure. The residue was purified by column chromatography on a silica gel (PE/EA, 2:1) to give compound PI-23b (2.1 g, 33%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,67853-03-6, Methyl 3-(hydroxymethyl)benzoate, and friends who are interested can also refer to it.

Reference:
Patent; Foresee Pharmaceuticals Co., Ltd.; YANG, Wenjin; CHANG, Kai-Wei; LIU, Suying; TSAI, Cheng-Han; (98 pag.)US2019/352288; (2019); A1;,
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Related Products of 101-98-4 ,Some common heterocyclic compound, 101-98-4, molecular formula is C10H15NO, 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.

Preparation 3A; Biphenyl-2-ylcarbamic Acid 1-[2-(Benzylmethylamino)ethyl]piperidin-4-yl Ester The title compound was prepared by mesylation of N-benzyl-N-methyl ethanolamine, which was then reacted with biphenyl-2-ylcarbamic acid piperidin-4-yl ester in an alkylation reaction. A 500 mL flask (reactor flask) was charged with N-benzyl-N-methylethanolamine (24.5 mL), DCM (120 mL), NaOH (80 mL; 30 wt %) and tetrabutylammonium chloride. Mixing at low speed throughout the reaction, the mixture was cooled to -10 C. (cooling bath), and the addition funnel charged with DCM (30 mL) and mesyl chloride (15.85 mL), which was added drop wise at a constant rate over 30 minutes. The addition was exothermic, and stirring was continued for 15 minutes while the temperature equilibrated back to -10 C. The reaction was held for at least 10 minutes to ensure full hydrolysis of the excess mesyl chloride. A 250 mL flask was charged with biphenyl-2-ylcarbamic acid piperidin-4-yl ester (26 g; prepared as described in Preparation 1) and DCM (125 mL), stirred for 15 minutes at room temperature, and the mixture chilled briefly to 10 C. to form a slurry. The slurry was then charged into the reactor flask via the addition funnel. The cooling bath was removed and the reaction mixture was warmed to 5 C. The mixture was transferred to a separatory funnel, the layers allowed to settle, and the aqueous layer removed. The organic layer was transferred back to the reactor flask, stirring resumed, the mixture held to room temperature, and the reaction monitored by HPLC for a total of 3.5 hours. The reactor flask was charged with NaOH (1M solution; 100 mL), stirred, and the layers allowed to settle. The organic layer was separated, washed (NaCl satd. solution), its volume partially reduced under vacuum, and subjected to repeated IPA washings. The solids were collected and allowed to air-dry (25.85 g, 98% purity). Additional solids were obtained from further processing of the mother liquor (volume reduction, IPA, cooling).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,101-98-4, its application will become more common.

Reference:
Patent; THERAVANCE, INC.; US2006/205775; (2006); A1;,
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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 1117-86-8, name is 1,2-Octanediol. This compound has unique chemical properties. The synthetic route is as follows. Safety of 1,2-Octanediol

General procedure: 2.2.1. General protocol A. The acylation of 1,2-alkanediols withacid chloride1,2-Alkanediol was dissolved in pyridine on slight heating;petroleum ether (PE) was added and the mixture was shaken untilhomogenization. Acid chloride was added dropwise on efcientmagnetic stirring. The mixture was stirred at RT for 0.25-16 hdepending on the target compound. Reaction was monitored byTLC. Methanol (0.5 ml) was added to the mixture when excessof acid chloride was used and stirring was continued for addi-tional 10 min. The reaction mixture was diluted with ethyl acetate(EtOAc) and aqueous NaHCO3 (10%) was added. Following the neutralization the water layer was separated, and the organic layerwashed twice with brine, dried over anhydrous MgSO4, ltered,concentrated and puried by ash chromatography over silica gel.(NB 1,2-Alkanediol bisbutyrates were used in preparative-scalelipase-catalyzed cleavage without previous purication.) The tar-get products were gained in 91-96% yields.;

With the rapid development of chemical substances, we look forward to future research findings about 1117-86-8.

Reference:
Article; Parve, Jaan; Reile, Indrek; Aid, Tiina; Kudrja?ova, Marina; Mueuerisepp, Aleksander-Mati; Vallikivi, Imre; Villo, Ly; Aav, Riina; Pehk, Tonis; Vares, Lauri; Parve, Omar; Journal of Molecular Catalysis B: Enzymatic; vol. 116; (2015); p. 60 – 69;,
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Adding a certain compound to certain chemical reactions, such as: 702-82-9, 3-Aminoadamantan-1-ol, 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, name: 3-Aminoadamantan-1-ol, blongs to alcohols-buliding-blocks compound. name: 3-Aminoadamantan-1-ol

A solution of 66.90 g of 3-amino-1-adamantanol and 340 ml of anhydrous methanol was added successively to 500 ml of 3-necked flask. After stirring, 46.74 g of benzaldehyde was added dropwise, and the mixture was heated and refluxed.After 3 hours, TLC (thin layer chromatography) monitored the reaction until complete conversion of the starting material to form the intermediate.After cooling the reaction system to 0 C, 18.2 g of sodium borohydride was added in portions to the reaction system.After the addition is complete, the reaction is carried out at 0 C to 5 C for 1 to 2 hours.After completion of the reaction by TLC (thin layer chromatography), the solvent was removed by rotary evaporation.To the residue was added 200 ml of water and 300 ml of ethyl acetate, and the organic phase was separated.The organic phase was washed twice with 100 ml of saturated brine, dried over anhydrous sodium sulfate and concentrated to remove the solvent. The crude product was obtained as an oil (118.1 g), which was recrystallized from petroleum ether / ethyl acetate (Volume ratio = 1: 1) to give 95.5 g of a white solid in 92.8% yield

The synthetic route of 702-82-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shandong Weizhi Medicine Industry Co. Ltd.; Wei, yanjun; Wang, hua; Meng, zhoujun; (12 pag.)CN103980175; (2016); B;,
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Application of 2050-25-1 , The common heterocyclic compound, 2050-25-1, name is 2-(2-(Benzyloxy)ethoxy)ethanol, molecular formula is C11H16O3, 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.

2-(2-(Benzyloxy)ethoxy)ethanol (5 g, 25.5 mmol) was dissolved in DCM (50 mE), passed through a phase separator and concentrated in vacuo. It was then redissolved in dry THF (50 mE, 25.5 mmol) under nitrogen and cooled in an ice bath. NaH (60% in mineral oil, 1.070 g, 26.8 mmol)was added portionwise over 10 mm and the resulting suspension stirred for 30 mm. Ethyl 2-bromopropanoate (3.73 mE, 28.0 mmol) was added dropwise over 15 mm. The reaction was stirred overnight, quenched with sat. NHa4C (5 mE) and the resulting mixture concentrated directly onto silica gel. The crude product was purified by chromatography on silica gel (80 g column, 0-50% EtOAc/isohexane) to afford the sub-title compound (1.51 g) as a colourless oil.?H NMR (400 MHz, DMSO-d6) oe 7.51-7.09 (m, 5H), 4.50 (s, 2H), 4.11 (qd, 2H), 4.05 (q, 1H), 3.70-3.41 (m, 8H), 1.27 (d, 3H), 1.20 (t, 3H)

The synthetic route of 2050-25-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Respivert Limited; Topivert Pharma Limited; FYFE, Matthew Colin Thor; THOM, Stephen Malcolm; (88 pag.)US2017/291917; (2017); A1;,
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Reference of 2043-47-2, Adding some certain compound to certain chemical reactions, such as: 2043-47-2, name is 1H,1H,2H,2H-Nonafluoro-1-hexanol,molecular formula is C6H5F9O, 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 2043-47-2.

Comparative Example 1In a 100-ml, three-necked glass reactor were placed 50 ml of methylene chloride, 10 g (38 mmol) of 3,3,4,4,5,5,6,6,6-nonafluorohexanol, 10 g (139 mmol) of acrylic acid, 0.1 g of a polymerization inhibitor, Sumilizer GM and 0.2 of toluenesulfonic acid. The mixture was heated. A reaction was allowed to proceed while distillation was made under normal pressure to remove the generated water together with methylene chloride. Every time when the amount of methylene chloride became small and the reactor-inside temperature exceeded 43 C., fresh methylene chloride was added into the reactor, to conduct the reaction for total 10 hours. At this point, the conversion was 82% and the selectivity was 84%.

According to the analysis of related databases, 2043-47-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; TOKUYAMA CORPORATION; DAIKIN INDUSTRIES, LTD.; US2009/23948; (2009); A1;,
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Reference of 30595-79-0, 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. 30595-79-0, name is 2,6-Dichlorophenethyl alcohol, molecular formula is C8H8Cl2O, 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.

Under the protection of argon, Weigh compound 5-2 (0.5 g, 2.62 mmol) in anhydrous toluene (8 mL), Add sodium hydride (0.131 g, 3.28 mmol), After heating to 40 C and stirring for 15 minutes, Cool the reaction to room temperature, Cuprous chloride (13 mg, 0.131 mmol) was added, Toluene (2 mL) and ethyl acetate (0.013 mL) were subsequently added, Heated to 120 C and refluxed for 24h, After the reaction is completed, the reaction solution is cooled to room temperature. Slowly add ice water to quench the sodium hydride, filter to remove insoluble matter, The filtrate was diluted with water and transferred to a separating funnel. Extract with methyl tert-butyl ether (10 mL x 3), combine the organic phases, The organic phase was washed with saturated brine (5 mL x 3), dried over anhydrous sodium sulfate, The solvent was distilled off under reduced pressure, The residue was purified by column chromatography (eluent: petroleum ether / ethyl acetate = 50: 1), Compound 5-3 (light yellow liquid, 0.25 g) was obtained.

According to the analysis of related databases, 30595-79-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; China Pharmaceutical University; Sun Hongbin; Kong Yi; Chen Si; Chen Panpan; Chen Fangjun; Song Hangyu; Ren Shenhong; Liu Zhaojun; (140 pag.)CN110627817; (2019); A;,
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Application of 17100-58-2, 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 17100-58-2, name is (4-Bromo-2-methylphenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows.

4-bromo-2-methyl-l-(phenoxymethyl) benzene. To a solution of (4-bromo-2- methylphenyl)methanol (1 g, 5 mmol), phenol (525 mg, 5.6 mmol) and triphenylphosphine (2.2 g, 8.4 mmol) in tetrahydrofuran (30 mL) was added diisopropyl azodicarboxylate (1.7 g, 8.4 mmol) at 0C. The mixture was stirred at 20C for 12 hours. Water (15 mL) was added to the mixture and then extracted with ethyl acetate (35 mL x 3). The combined organic phase was dried by sodium sulfate, and then filtered. The filtrate was concentrated in vacuo and the residue was purified by column chromatography (silica gel, petroleum ether/ethyl acetate = 5:1) to give 4-bromo-2-methyl-l-(phenoxymethyl) benzene (640 mg, 46%).

According to the analysis of related databases, 17100-58-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; CONSTELLATION PHARMACEUTICALS; ALBRECHT, Brian, K.; AUDIA, James, Edmund; COOK, Andrew; GAGNON, Alexandre; HARMANGE, Jean-christophe; NAVESCHUK, Christopher, G.; WO2013/75083; (2013); A1;,
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Electric Literature of 486460-26-8, 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 486460-26-8, name is (4-Bromo-2,5-difluorophenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows.

To a solution of 2 g (8.44 mmol) of 4-bromo-2,5-difluorobenzoic acid (prepared according to the procedure of Ishikawa et al., Kogyo Kagaku Zasshi, pg 972-979, 1970) in 20 mL of tetrahydrofuran was added 40 mL of a 1M solution of borane-tetrahydrofuran complex. The solution was heated under reflux for 64 h, cooled to ambient temperature and 100 mL of methanol was added. The reaction was then heated for a further 2 h, cooled and concentrated in vacuo. Purification by flash chromatography (silica gel, 9:1 hexane:ethyl acetate) afforded 1.6 g of 4-bromo-2,5-difluorobenzyl alcohol. To a solution of 1.3 g (5.6 mmol) of 4-bromo-2,5-difluorobenzyl alcohol in 20 mL of dichloromethane at 0 C. was added 2.27 g (6.7 mmol) of carbon tetrabromide and 1.8 g (6.7 mmol) of triphenylphosphine. The reaction was stirred for 2 h at this temperature, the solvent was removed in vacuo and the residue stirred with 100 mL of diethyl ether. The solution was filtered, concentrated in vacuo, and purified by flash chromatography (silica gel, 9:1 hexane:ethyl acetate) to afford 1.5 g of the title compound.

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 486460-26-8, (4-Bromo-2,5-difluorophenyl)methanol.

Reference:
Patent; Merck Sharp & Dohme Corp.; Edmondson, Scott D.; Fisher, Michael H.; Kim, Dooseop; Maccoss, Malcolm; Parmee, Emma R.; Weber, Ann E.; Xu, Jinyou; US2015/359793; (2015); A1;,
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