Alcohols-buliding-blocks

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 623-72-3 as follows., 623-72-3

Example 16 This example describes the preparation of various alkyl acrylate esters by dehydrating 3-HP esters using various catalysts. A catalyst was placed in a 3-neck flask that was equipped with a temperature probe (in contact with the catalyst). A distillation column and receiving flask were attached so that the vapors formed during the reaction could be collected, and the catalyst was heated to the desired temperature. A solution of a 3-hydroxypropionic acid ester in the corresponding alcohol was added drop-wise directly onto the catalyst using a syringe. The liquid that distilled over was collected and analyzed by gas chromatography. The results, and corresponding experimental conditions are shown in the following table. Ester Catalyst Temperature Concentration Solvent Yield of Yield of (C) of Ester in Acrylic Acrylic Solvent ester (GC) acid (GC) – (%) (%) (%) Ethyl NaH2P04-Silica 275-EtOH 49 26 Ethyl NaH2PO4-Silica 250 35 EtOH 53 Ethyl NaH2PO4-Silica 250 50 EtOH 14 21 Ethyl NaH2PO4-Silica 180 40 EtOH 30 – Ethyl Copper-H3PO4 220 20 EtOH 50 50 Methyl NaH2PO4-Silica 280-MeOH 78 Methyl CuS04-Silica 280-MeOH 37 9 Methyl Cs2CO3-Silica 220 45 MeOH 49 – Butyl NaH2PO4-Silica 280 50 BuOH 40 Similar dehydration reactions were performed using 3-HP as the starting material and a flask containing heated catalyst in place of the GC: (a) Aqueous 3-HP was dehydrated to acrylic acid over NaH2PO4-Silica gel catalyst at 180C. Based on GC and HPLC analysis, the yield of acrylic acid was 90- 96%. (b) Aqueous 3-HP was dehydrated to acrylic acid over H3PO4-Silica gel catalyst at 180C. Based on GC and HPLC analysis, the yield of acrylic acid was 85-90%. (c) Aqueous 3-HP was dehydrated to acrylic acid over CuS04-Silica gel catalyst at 180C. Based on GC and HPLC analysis, the yield of acrylic acid was 73%. (d) Aqueous 3-HP was dehydrated to acrylic acid over Zeolite H-ss powder and 85% H3PO4 as the catalyst at 180C. Based on GC and HPLC analysis, the yield of acrylic acid was 71%. (e) Aqueous 3-hydroxyisobutyric acid was dehydrated to methacrylic acid over NaH2PO4-Silica gel catalyst at 270C. Based on GC analysis, the yield of methacrylic acid was 79%.

The chemical industry reduces the impact on the environment during synthesis 623-72-3, I believe this compound will play a more active role in future production and life.

Reference:
Patent; CARGILL, INCORPORATED; WO2003/82795; (2003); A2;,
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647-42-7 ,Some common heterocyclic compound, 647-42-7, molecular formula is C8H5F13O, 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 solution of TsCl (8.24212 mmol, 1 equiv) or MsCl (8.24 mmol, 1 equiv) in DCM (24 mL) was added dropwise to a stirred solution of fluorinated alcohol 1-5 (8.24 mmol, 1 equiv) and Et3N (1.78 mL, 1.55 equiv) at 0 C. After complete addition (10 min) the reaction mixture was allowed to reach rt and stirring was continued overnight. Then, the reaction mixture was washed with H2O (34 mL) and brine (34 mL). The organic layer was dried over Na2SO4 and concentrated to dryness under reduced pressure. The resulting crude product was crystallized from MeOH to afford 1a-5b.

According to the analysis of related databases, 647-42-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Tomaszewska, Joanna; Koroniak-Szejn, Katarzyna; Koroniak, Henryk; Arkivoc; vol. 2017; 2; (2016); p. 421 – 432;,
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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. 558-42-9, name is 1-Chloro-2-methyl-2-propanol. A new synthetic method of this compound is introduced below., 558-42-9

INTERMEDIATE 13; (3R.6S)-3-Amino-6-(‘2.3-difluorophenylVl-(2-hydroxy-2-methylpropyl’)azepan-2-one; Step A. Di-fert-butyl r(3R.66f)-6-(;2.3-difluorophenylVl-(;2-hvdroxy-2-methylpropylV2-oxoazepan-3- yl] imidodicarbonate; A solution of (55)-N2,N2-bis(tert-butoxycarbonyl)-5-(2,3-difluorophenyl)-D-lysine (0.569 g, 1.24 mmol), l-chloro-2-methyl-2-propanol (0.202 g, 1.86 mmol) and diisopropylethylamine (0.529 g, 4.10 mmol) in EtOH (5 mL) was heated at 75 0C overnight. The reaction was concentrated to dryness, diluted with DCM (20 mL) and EDC (0.358 g, 1.87 mmol), HOAT (0.252 g, 1.87 mmol) were added followed by diisopropylethylamine (0.650 mL, 3.73 mmol). After stirring overnight, NaHCO3 was added, the layers separated and the aqueous phase backwashed with DCM. The combined organics were dried over magnesium sulfate, filtered, concentrated and the residue purified by silica gel chromatography (10percent –> 35percent EtOAc / hexanes) to give the title compound (0.21 g). MS 513.1 (M+l). 1HNMR (500 MHz, CD3OD) delta 7.1 (m, 3H), 5.24 (d, J= 10.7 Hz, IH), 4.02 (m, IH), 3.69 (d, J= 13.9 Hz, IH), 3.60 (d, EPO J= 15.1 Hz, IH), 3.39 (m, IH), 3.24 (d, J= 14.2 Hz, IH), 2.4 (m, IH), 2.1 (m, 3H), 1.5 (s, 18H), 1.20 (s, 3H), 1.16 (s, 3H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,558-42-9, 1-Chloro-2-methyl-2-propanol, and friends who are interested can also refer to it.

Reference:
Patent; MERCK & CO., INC.; WO2006/41830; (2006); A2;,
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124-68-5, 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. 124-68-5, name is 2-Amino-2-methyl-1-propanol. A new synthetic method of this compound is introduced below.

General procedure: 2-Amino-2-methylpropanol (6, 4.89 g, 55 mmol, 8.5 eq),6.50 mmol of carbonyl compound 4 (1 eq), and 50 mg of H2-activated clay are placed in an autoclave (100 cm3).The sealed reactor is heated for 24 h at various temperatures.After cooling and separation of the H2-clay by filtration,the residue is treated in the same manner asdescribed above. The yields of oxazolidines 7 are given inTable 5.

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:
Article; Rohand, Taoufik; Savary, Jerome; Marko, Istvan E.; Monatshefte fur Chemie; vol. 149; 8; (2018); p. 1429 – 1436;,
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Adding some certain compound to certain chemical reactions, such as: 6338-55-2, name is 2-(2-(2-Aminoethoxy)ethoxy)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 6338-55-2. 6338-55-2

A solution of the amino alcohol (20) (313.6 g, 2.1mol) in THF (3.5 L) was treated, portion-wise, with N-(Benzyloxycarbonyloxy)succinimide (21) (550 g, 2.21mol). Once the reaction was complete (18 h) the THF was removed under reduced pressure and the residue dissolved in CH2Cl2 (2.5 L), then washed with an equal volume of HCl (1 M), NaHCO3 (Sat. Aq.), H2O and brine. The organic extract was dried (MgSO4), filtered and concentrated. The crude material (600g) was subjected to chromatography (4kg silica; 1-12% CH3OH-CH2Cl2) to yield HO-Trig- NHZ (22) (468g, 78%) as a clear-yellow viscous oil

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 6338-55-2.

Reference:
Patent; ARBUTUS BIOPHARMA CORPORATION; HEYES, James; HOLLAND, Richard J.; PALMER, Lorne Ralph; WOOD, Mark; (0 pag.)WO2020/93053; (2020); 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 2854-16-2, name is 1-Amino-2-methylpropan-2-ol. This compound has unique chemical properties. The synthetic route is as follows. 2854-16-2

5-(2 ,4-dichloro-5-(3-fluoropyridin-2-yl)benzamido)- 1 -phenyl- 1 H-pyrazole-3-carboxylicacid (Example 107, 78 g, 166 mmol) was sonicated in DMF (300 mL) with N,Ndiisopropylethylamine (58 mL, 332 mmol) to give a clear solution, which was cooled to 10CC. TPTU (74 g, 249 mmol) was added portionwise and the mixture stirred at 10C for20 minutes. A solution of 1-amino-2-methylpropan-2-ol (22.1 g, 249 mmol) in DMF (50 mL) was added dropwise at 1000 and the mixture then allowed to warm to room temperature and stirred for 16 hours. The reaction mixture was partitioned between EtOAc (600 mL) and water (600 mL). The aqueous layer was separated and extracted with additional EtOAc (3 x 200 mL). The combined organic layers were washed withsaturated aqueous ammonium chloride solution (300 mL), water (5 x 200 mL), dried (magnesium sulphate) and concentrated in vacuo to give an orange oil. The oil was treated with acetonitrile (300 mL) and the resulting solid collected by filtration, washed with acetonitrile and dried under vacuum to afford the title compound as a colourless solid (60 g, 66%).1H NMR (400MHz, DMSO-d6): O ppm 1.09 (s, 6H), 3.21-3.22 (d, 2H), 4.63 (5, 1H), 6.93(5, 1H), 7.45-7.49 (m, 1H), 7.50-7.55 (t, 2H), 7.58-7.65 (m, 3H), 7.69 (5, 1H), 7.80-7.85(t, 1H), 7.87-7.95 (m, 2H), 8.56-8.58 (d, 1H), 10.89 (5, 1H).MS m/z 540.45 [M-Hr

Statistics shows that 2854-16-2 is playing an increasingly important role. we look forward to future research findings about 1-Amino-2-methylpropan-2-ol.

Reference:
Patent; PFIZER INC.; BAGAL, Sharanjeet Kaur; CUI, Jingrong Jean; GREASLEY, Samantha Elizabeth; LUNNEY, Elizabeth Ann; MCALPINE, Indrawan James; NAGATA, Asako; NINKOVIC, Sacha; OMOTO, Kiyoyuki; SKERRATT, Sarah Elizabeth; STORER, Robert Ian; WARMUS, Joseph Scott; WO2015/170218; (2015); 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 6338-55-2, name is 2-(2-(2-Aminoethoxy)ethoxy)ethanol. This compound has unique chemical properties. The synthetic route is as follows. 6338-55-2

4-Ethynylaniline (170.4 mg, 1.5 mmol) was added to a solution of 4-nitrophenyl chloroformate (289.3 mg, 1.4mmol) in tetrahydrofuran (6.8 mL), stirred at room temperature for 3 hours, and then the solvent was distilled away undera reduced pressure. To a solution of the resulting crude product in dichloromethane (4 mL), a solution of 2-[2-(2-aminoethoxy)ethoxy]ethanol (239 mg, 1.6 mmol) in dichloromethane (4 mL) and triethylamine (303 mL, 2.2 mmol) wereadded, stirred at room temperature overnight, and then the solvent was distilled away under a reduced pressure. Theresidue was purified by silica gel column chromatography (ethyl acetate/methanol (v/v) = 100/0 ? 90/10) to obtain thetitle compound (325.4 mg, 77%) as a pale yellow oily matter.1H NMR (400 MHz, CDCl3) delta 8.30 (1H, br s), 7.32 (4H, m), 6.22 (1H, br t, J = 4.4 Hz), 4.37 (1H, br s), 3.72 (2H, br t, J= 4.4 Hz), 3.55-3.53 (6H, m), 3.49 (2H, t, J = 4.4 Hz), 3.36-3.34 (2H, m), 3.05 (1H, s)

Statistics shows that 6338-55-2 is playing an increasingly important role. we look forward to future research findings about 2-(2-(2-Aminoethoxy)ethoxy)ethanol.

Reference:
Patent; Senju Pharmaceutical Co., Ltd.; TAKEDA, Norihiko; MIYABE, Tomoyo; MACHIDA, Shinnosuke; MACHIDA, Mamiko; NAKAJIMA, Takeshi; (94 pag.)EP3127900; (2017); A1;,
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1074-16-4, 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 1074-16-4, name is 2-(2-Bromophenyl)ethanol. This compound has unique chemical properties. The synthetic route is as follows.

17.6 g (0.314 mol) KOH in 100 mL DMSO was placed in a flask fitted with dropping funnel and magnetic stirrer placed in water bath at ca. 7 C. A solution of 9.9 mL (22.57 g, 0.159 mol) of iodomethane and 13.94 g (0.0742 mol) of 2-(2-bromophenyl)ethanol in 80 mL DMSO was dropped-in while keeping the temperature 21-22 C. Water bath was removed and the reaction mixture was stirred for 2 h while the temperature raised to 27 C. After cooling to RT reaction mixture was poured into 600 mL of water, than extracted with diethyl ether (300 mL and 2 ¡Á 100 mL). Ether extract was washed with water (2 ¡Á 150 mL) and volatiles were distilled off to give 14.6 g of 2-bromo-(2-methoxyethyl)benzene (0.0679 mol, 91.5%), which was used without further purification. 1H NMR (400 MHz, CDCl3): delta: 3.08 (t, 2H), 3.42 (s, 3H), 3.66 (t, 2H), 7.10-7.14 (m, 1H), 7.26-7.33 (m, 2H), 7.57-7.59 ppm (m, 1H).

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 1074-16-4, 2-(2-Bromophenyl)ethanol.

Reference:
Article; Adamczyk-Wo?niak, Agnieszka; Brzozka, Zbigniew; Da?browski, Marek; Madura, Izabela D.; Scheidsbach, Roy; Tomecka, Ewelina; Zukowski, Kamil; Sporzy?ski, Andrzej; Journal of Molecular Structure; vol. 1035; (2013); p. 190 – 197;,
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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. 764-48-7, name is Ethylene Glycol Vinyl Ether. This compound has unique chemical properties. The synthetic route is as follows. 764-48-7

General procedure: A dry and argon-flushed 10 mL Schlenk tube, equipped with a stirring bar and septum, wascharged with 2-(vinyloxy)ethanol (5, 132 mg, 1.50 mmol, 1.50 equiv) in Et2O (1.5 mL). Then,iPrMgBr (1.55 mmol, 1.55 equiv) was added dropwise at 25 C. After 5 min of stirring,Sc(OTf)3 (49.2 mg, 0.10 mmol, 0.10 equiv) and aldehyde 6 (1.00 mmol, 1.00 equiv) weresuccessively added and the reaction mixture was stirred at 40 C for the given time. After afull conversion was detected by GC-analysis, sat. aq. NH4Cl (15 mL) was added and theaqueous layer was extracted with EtOAc (3 x 15 mL). The combined organic layers weredried over Na2SO4, filtered and solvent was removed under reduced pressure. Purification viacolumn chromatography (SiO2) afforded expected products 4.

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, 764-48-7, Ethylene Glycol Vinyl Ether.

Reference:
Article; Quinio, Pauline; Kohout, Laura; Roman, Daniela Sustac; Gaar, Jakob; Karaghiosoff, Konstantin; Knochel, Paul; Synlett; vol. 27; 11; (2016); p. 1715 – 1719;,
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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.932-01-4, name is 4,4-Dimethylcyclohexanol, molecular formula is C8H16O, molecular weight is 128.21, as common compound, the synthetic route is as follows.932-01-4

(3) N,N’-carbonyldiimidazole (118 mg) was added to a mixture of 4,4-dimethylcyclohexanol (72 mg) and acetonitrile (7 ml). The reaction mixture was stirred at 45 C. for 1 hour, added with water and chloroform and washed with water. The organic layer was dried over sodium sulfate and the solvent was evaporated under reduced pressure. The product (190 mg) of the above (2), triethylamine (0.21 ml), 4-dimethylaminopyridine (10 mg) and DMF (5 ml) were added to the residue and the reaction mixture was heated at 80 C. for 1 hour. The reaction mixture was evaporated under reduced pressure, and water and chloroform were added thereto. The organic layer was dried over sodium sulfate and the solvent was evaporated under reduced pressure. The residue was purified by silica gel chromatography (elution solvent: hexane/ethyl acetate=100/0 to 0/100 gradient) to obtain 135 mg of 4,4-dimethylcyclohexyl (S)-3-(4-benzyloxy-3-methoxybenzylcarbamoyl)-piperidine-1-carboxylate.

Statistics shows that 932-01-4 is playing an increasingly important role. we look forward to future research findings about 4,4-Dimethylcyclohexanol.

Reference:
Patent; Tsuzuki, Yasunori; Morie, Toshiya; Nakamura, Takanori; Shimizu, Isao; Miyauchi, Masanori; US2012/28937; (2012); A1;,
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