Author: tianli

Reference of 135241-08-6, 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 135241-08-6 as follows.

the above-mentioned 4-chloro-1-hydroxy-naphthalene carboxylic acid methyl ester 32g of triflic anhydride 68g were dissolved and stirred at room temperature for 6 hours in 400ml of pyridine. 500ml After adding water, using a separatory funnel, and extracted with toluene 500ml. 3333 Further organic layer was washed with pure water three times, the use of dilute aqueous hydrochloric acid The organic layer was washed three times using aqueous sodium bicarbonate The organic layer was washed three times, then the organic layer was washed with pure water three times. The organic layer was collected and dried over anhydrous magnesium sulfate. After filtration over anhydrous magnesium sulfate, and concentrated using a rotary evaporator to obtain a crude product. 4–1-(((20g( 40% ) The crude product with heptane were recrystallized, thereby obtaining the following 4-chloro-1 – (((trifluoromethyl) sulfonyl) hydroxy) naphthalene carboxylate 20g (yield: 40%)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,135241-08-6, its application will become more common.

Reference:
Patent; JNC Co., Ltd.; Kageyama, Akiko; (341 pag.)KR2015/74015; (2015); A;,
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Reference of 403-41-8, 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. 403-41-8, name is 1-(4-Fluorophenyl)ethyl Alcohol. A new synthetic method of this compound is introduced below.

0039] H Equipped with a magnetic stirrer in round bottom flask methyl benzyl alcohol (12. 22g, 100. Ommol, namely formula The R1 is 4-methyl, R2 is hydrogen, X is carbon, eta is 1, m is 0), ferric chloride (0. 81g, 5mmol), L- isoleucineAcid (1.31g, 10mmol), TEMP0 (1.56g, 10mmol), toluene 300. OmL was added , then the reaction with oxygen in the air bottleReplacement, stirred and reflux for 6h. After completion of reaction, the reaction mixture was cooled to room temperature, filtered, the filtrate evaporated to give the crude product,The resultant crude product was purified by column chromatography, with n-hexane: Elution: (10 1 volume ratio) mixed liquid of ethyl acetate containing the desired collectionLabeled compound of the eluent, evaporation of the solvent and dried to give the product p-tolualdehyde 10. 93g, 91% yield. 1- (4-fluorophenyl) ethanol (1 · 40g, 10. Ommol, i.e., of formula (I), R1 is 4-fluoro,R2 is methyl, X is carbon, [eta] is l, m is 0) is used, experimental methods and procedures were the same as in Example 1, except that: trifluoromethanesulfonate Iron(0 · 50g, 1. Ommol), L- isoleucine (0 · 26g, 2 · Ommol), TEMPO (0 · 16g, 1 · Ommol), xylene 30. OmL,After stirring at reflux with oxygen reaction bottle of air displacement 48h. To give the final product 1.23g, 88% yield.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,403-41-8, 1-(4-Fluorophenyl)ethyl Alcohol, and friends who are interested can also refer to it.

Reference:
Patent; Zhejiang University; Zhang, Guofu; Li, Shasha; Ding, Chengrong; Zhang, Guihua; Xie, Xiaoqiang; Lei, Jie; (12 pag.)CN105294413; (2016); A;,
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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 44565-27-7, name is 4-Amino-2-methylbutan-1-ol. This compound has unique chemical properties. The synthetic route is as follows. Recommanded Product: 44565-27-7

Reference Example 17 (+/-)-N-[3,5-Bis(trifluoromethyl)benzyl]-7,8-dihydro-7-(4-hydroxy-3-methylbutyl)-5-(4-methylphenyl)-8-oxo-6-pyrido[3,4-b]pyridinecarboxamide The compound as obtained in Reference Example 3 was reacted with 4-amino-2-methyl-1-butanol and treated in the same manner as in Reference Example 13, to obtain the entitled compound as colorless crystals. m.p. 129-130 C. (after once melted, this again solidified), 188-190 C. (re-melted) (recrystallized from ethyl acetate-isopropyl ether) NMR(200 MHz, CDCl3) ppm: 0.79(3H,d,J=6.6 Hz), 1.4-1.8(3H,m), 2.28(3H,s), 3.03(1H,t,J=6.6 Hz,-OH), 3.2-3.7(4H,m), 4.49(2H,d,J=5.8 Hz), 7.0-7.3(4H,m), 7.30(1H,dd,J=8.4,4.4 Hz), 7.53(1H,dd,J=8.4,1.4 Hz), 7.68(2H,s), 7.78(1H,s), 8.48(1H,t,J=6.0 Hz), 8.61(1H,dd,J=4.4,1.4 Hz).

With the rapid development of chemical substances, we look forward to future research findings about 44565-27-7.

Reference:
Patent; Natsugari, Hideaki; Doi, Takayuki; Ikeura, Yoshinori; US2002/132817; (2002); A1;,
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Adding a certain compound to certain chemical reactions, such as: 111-46-6, 2,2′-Oxybis(ethan-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, Computed Properties of C4H10O3, blongs to alcohols-buliding-blocks compound. Computed Properties of C4H10O3

2,2-oxydiethanol (168 mmol) in THF (100 ml) was added dropwise to a solution of sodium hydride (42mmol) in THF (80 ml) at 0C during 30 minutes. The solution was stirred for 2 hours at room temperature. 3-bromoprop-1-yne (42 mmol) was added and the solution was refluxed overnight, followed by addition of water (80 ml). Solvent was evaporated and extracted with EtOAc (4x lOOmI). The combined organic layers were washed with brine, dried over anhydrous Na2504, filtered and concentrated in vacuo. The obtained mixture was purified with flash chromatography (100% Heptaneto 40% EtOAc in Heptane)Yield: 58.3 %, MS (ESI) m/z 167 [M+Na] +1H-NMR (ODd3, 400 MHz) 6 2.44 (t, J=2.4 Hz, 1H), 3.62 (t, J=4.4 Hz, 2H), 3.69-3.77 (m, 6H), 4.22 (d, J=2.4Hz, 2H)

The synthetic route of 111-46-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; UNIVERSITEIT ANTWERPEN; JOOSSENS, Jurgen; AUGUSTYNS, Koen; LAMBEIR, Anne-Marie; VAN DER VEKEN, Pieter; VAN SOOM, Jeroen; MAGDOLEN, Viktor; (66 pag.)WO2015/144933; (2015); A1;,
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Reference of 60666-70-8 , The common heterocyclic compound, 60666-70-8, name is (2-Bromo-5-chlorophenyl)methanol, molecular formula is C7H6BrClO, 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.

General procedure: A DMF solution (8mL) of the o-substituted aryl iodide (0.36mmol), the o-bromobenzyl alcohol (0.36mmol) and norbornene (34mg, 0.36mmol) was added under nitrogen to a Schlenck-type flask, containing Pd(OAc)2 (4mg, 0.018mmol), the phosphine (0.036mmol), when required, and K2CO3 (124mg, 0.90mmol) or CsOPiv (211mg, 0.90). The reaction mixture was stirred at 105°C for 24h. After cooling to room temperature the organic layer was diluted with EtOAc (20mL), washed twice with water (20mL) and dried over Na2SO4. The solvent was removed under reduced pressure and the resulting residue was purified by flash chromatography on silica gel using mixtures of hexane-EtOAc as eluent.

The synthetic route of 60666-70-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Della Ca, Nicola; Fontana, Marco; Xu, Di; Cremaschi, Mirko; Lucentini, Riccardo; Zhou, Zhi-Ming; Catellani, Marta; Motti, Elena; Tetrahedron; vol. 71; 37; (2015); p. 6389 – 6401;,
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Synthetic Route of 78573-45-2, 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.78573-45-2, name is 3-(3-(Trifluoromethyl)phenyl)propan-1-ol, molecular formula is C10H11F3O, molecular weight is 204.19, as common compound, the synthetic route is as follows.

10 kg of dichloromethane was added to a 50 L reactor, and 3-(3-trifluoromethylphenyl)propanol (1 kg, 4.90 mol) and triethylamine (0.59 kg, 5.88 mol) were added in sequence with stirring. The jar was rinsed with 3 kg of dichloromethane. Cool down to -5-10 C, Methanesulfonyl chloride (0.62 kg, 5.39 mol) was slowly added dropwise. The temperature of the reaction system was maintained at -5 to 10 C, and the addition was completed at about 50 to 80 minutes. The incubation was continued until the TLC monitoring reaction was complete and the reaction was completed in about 1 h. 10 kg of water was added under stirring, stirring was continued for 20 min, and the layers were allowed to stand. The organic phase was retained, and the aqueous phase was further extracted with 11 kg of dichloromethane. The organic phase was combined and the aqueous phase was discarded. The organic phase was transferred to a 50 L reactor, cooled to 5-10 C, 10 kg of water was added, stirred for 30 min, allowed to stand for stratification, and the aqueous phase was discarded; the organic phase was washed with 10 kg of 10% NaCl solution, allowed to stand for stratification, and the water phase was discarded. go with. The organic phase was dried over 0.50 kg anhydrous magnesium sulfate and stirred for about 1 h. The magnesium sulfate was filtered off, the reaction kettle was rinsed with 2 kg of dichloromethane and the filter cake was washed, and the organic phases were combined. Transfer the organic phase to the concentrator, Concentrated under reduced pressure to give a yellow oily liquid 1.41kg. HPLC purity: 98.58%.

The chemical industry reduces the impact on the environment during synthesis 78573-45-2, I believe this compound will play a more active role in future production and life.

Reference:
Patent; Jiangsu Yong’an Pharmaceutical Co., Ltd.; Luo Huan; Kang Yanlong; Li Qian; Qiu Chunfang; Liu Kelei; Wang Shuaiwei; (8 pag.)CN109096119; (2018); A;,
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Reference of 4654-39-1, 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.4654-39-1, name is 2-(4-Bromophenyl)ethanol, molecular formula is C8H9BrO, molecular weight is 201.06, as common compound, the synthetic route is as follows.

1.31.a. 2-[2-(4-bromo-phenyl)-ethoxy]-tetrahydro-pyran 0.025 g of p-toluenesulphonic acid and 2.575 ml (28.22 mmol) of dihydropyran are added successively to a solution of 4.83 g (24.02 mmol) of 2-(4-bromo-phenyl)-ethanol in 12 ml dichloromethane at 0 C. Then the reaction mixture is stirred for three hours at ambient temperature. The reaction mixture is extracted with sodium hydrogen carbonate solution and the organic phase is dried over sodium sulphate. The purification is carried out by column chromatography on Alox (eluant: cyclohexane/ethyl acetate=8:2). Yield: 37 g (32.8% of theory); C13H17BrO2 (M=285.18); calc.: molar peak (M)+: 284/286 fnd.: molar peak (M)+: 284/286.

Statistics shows that 4654-39-1 is playing an increasingly important role. we look forward to future research findings about 2-(4-Bromophenyl)ethanol.

Reference:
Patent; Boehringer Ingelheim International GmbH; US2004/242572; (2004); 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. 23783-42-8, name is 2,5,8,11-Tetraoxatridecan-13-ol. This compound has unique chemical properties. The synthetic route is as follows. name: 2,5,8,11-Tetraoxatridecan-13-ol

Tetraethyleneglycol monomethyl ether (1 .91 ml, 9 mmol) dissolved in dry and degassed DMF (3.5 ml, dried 24 h, 4A MS) was added carefully to sodium hydride (365 mg, 9 mmol) in dry and degassed DMF (15 ml, dried 24 h, 4A MS) under nitrogen at 0 C using a syringe. The temperature was then raised to room temperature and the reaction mixture was stirred for another 30 min. 3-(3-bromo-2,2-bis(bromomethyl)propoxy)prop-1 -ene (730 mg, 2.0 mmol) was then added and the temperature was raised to 100 C. After 14 h the reaction was completed (HPLC-ELSD-C18, 95:5 to 5:95 H2O/ACN in 25 min, Rt product = 19.5 min) the temperature was decreased to room temperature and the reaction mixture was carefully added to H2O (150 ml) and the H2O-phase was washed with diethyl ether (2 x 50 ml). Sodium chloride was then added to the H2O-phase until saturation. The H2O-phase was extracted with EtOAc (4 x 50 ml) and the combined organic phases were washed with brine (2 x 30 ml). Sodium sulfate and charcoal was added to the organic phase. The clear organic phase was filtered and the volatile material was removed at reduced pressure (8 mm Hg, 40 C then 0.1 mm Hg (oil pump) and 40 C to remove residual DMF). Column chromatography (EtOAc:MeOH 9:1 ) gave 1 .05 g (70%) of the product. 1H-NMR (CDCI3); 5.90 (m, 1 H), 5.20 (m, 2H), 3.94 (dt, 2H), 3.70-3.55 (m, 48H), 3.45 (s, 6H), 3.43 (s, 2H), 3.40 (s, 9H).

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, 23783-42-8, 2,5,8,11-Tetraoxatridecan-13-ol.

Reference:
Patent; SPAGO IMAGING AB; AXELSSON, Oskar; PETORAL JR., Rodrigo M.; EK, Fredrik; LAURITZSON, Petter; WO2013/41623; (2013); A1;,
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Synthetic Route of 14002-80-3, Adding some certain compound to certain chemical reactions, such as: 14002-80-3, name is Methyl 3-hydroxy-2,2-dimethylpropanoate,molecular formula is C6H12O3, 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 14002-80-3.

[0417] Synthesis of methyl 2,2-dimethyl-3-oxopropanoate (91A): To a suspension of methyl 2,2-dimethyl-3-hydroxypropionate (1.93 ml, 15.1 mmol) and trichloroisocyanuric acid (3.52 g, 15.1 mmol) in dichloromethane (30 ml) was added TEMPO (50 mg, 0.3 mmol) at 0 C. The reaction was warmed to room temperature and stirred for 3 hours. The mixture was filtered and the filtrate was washed with 1M sodium bicarbonate (30mL), followed by 1M HC1 (30 mL), and brine (30 mL). The organic layer was dried with sodium sulfate, filtered, and concentrated under vacuum. The crude product was taken to the next step without further purification.

According to the analysis of related databases, 14002-80-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GILEAD SCIENCES, INC.; BRIZGYS, Gediminas; CANALES, Eda; HALCOMB, Randall, L.; HU, Yunfeng, Eric; KATO, Darryl; LINK, John, O.; LIU, Qi; SAITO, Roland, D.; TSE, Winston, C.; ZHANG, Jennifer, R.; (253 pag.)WO2016/33243; (2016); A1;,
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Reference of 1454-85-9, Adding some certain compound to certain chemical reactions, such as: 1454-85-9, name is Heptadecan-1-ol,molecular formula is C17H36O, 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 1454-85-9.

General procedure: To a cooled (0 C) solution of alcohol(1.0 mmol) in anhydrous dichloromethane (5 ml), triethylamine (2.0 mmol),methoxyacetyl chloride (1.5 mmol) and dimethylaminopyridine (0.1 mmol)were added. The reaction mixture was stirred for 12?16 h at rt. The reactionmass was diluted with water and extracted with dichloromethane. The organiclayer was washed with 1 N HCl, saturated sodium bicarbonate, brine and driedover anhydrous sodium sulphate. The solvent was evaporated and purificationwas carried out by flash column chromatography.

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. 1454-85-9, Heptadecan-1-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Gadekar, Pradip K.; Hoermann, Maryann; Corbo, Faith; Sharma, Rajiv; Sarveswari; Roychowdhury, Abhijit; Tetrahedron Letters; vol. 55; 2; (2014); p. 503 – 506;,
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