Month: August 2021

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 616-29-5, name is 1,3-Diaminopropan-2-ol, the common compound, a new synthetic route is introduced below. category: alcohols-buliding-blocks

Preparation of (3-tert-Butoxycarbonylamino-2-hydroxy-propyl)-carbamic Acid Tert-Butyl Ester: To a solution of 1,3 diamino-2-hydroxypropane (10 g, 0.11 mol) in methanol (500 ml) was added di-tert-butyl dicarbonate (48 g, 0.22 mumol) and the reaction stirred for 2 hours at room temperature under a N2 atmosphere. The mixture was concentrated to afford the product as a light yellow oil (31.9 g, 100%). 1H-NMR (CD3OD) delta 1.44 (s, 18H), 3.10 (m, 4H), 3.63 (m, 1H).

The synthetic route of 616-29-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bridger, Gary; Kaller, Al; Harwig, Curtis; Skerlj, Renato; Bogucki, David; Wilson, Trevor R.; Crawford, Jason; McEachern, Ernest J.; Atsma, Bem; Nan, Siqiao; Zhou, Yuanxi; Schols, Dominique; Smith, Christopher D.; Di Fluri, Maria R.; US2004/19058; (2004); A1;,
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In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 597-31-9, name is 3-Hydroxy-2,2-dimethylpropanal, the common compound, a new synthetic route is introduced below. Product Details of 597-31-9

The hydroxypivalaldehyde and sodium hydroxide solution obtained in the step (3) were added to a four-necked flask, heated and refluxed for 2 hours with stirring at 85 to 95 C,The weight ratio of the BaO / SiO2 core-shell microsphere catalyst was 27: 5: 270: 15, the weight ratio of the catalyst was 4: Stirring to 60 C while adding ammonia to keep the pH of the reaction solution 7-9, 8 hours after the stop reaction, the reaction solution suction filter, the filtrate concentration adjusted with concentrated hydrochloric acid ph value 3-4, extracted with acetone , After evaporation of acetone standing, precipitation crystallization is hydroxy pivalic acid, the yield was 91%

The synthetic route of 597-31-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Suzhou Yi Dike Pharmaceutical Chemical Co; Hu, Haiwei; Ding, Jing; Yan, Yongping; Zheng, Hui; Yan, Hui; (7 pag.)CN105753684; (2016); A;,
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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. 13330-96-6, name is 4-(Dimethylamino)butan-1-ol. A new synthetic method of this compound is introduced below., category: alcohols-buliding-blocks

A mixture of 2-hydroxy-4-({[3-(2-methyl-1,3-thiazol-4-yl)phenyl]sulfonyl}amino)benzoic acid (26 mg, 67 mumol), 4-(dimethylamino)-1-butanol (78 mg, 0.67 mmol), 4-dimethylaminopyridine (2.4 mg, 20 mumol) and N,N’-dicyclohexylcarbodiimide (41 mg, 0.20 mmol) was stirred in THF (1 ml) overnight at room temperature and further at 60 C. for 3 h. The solvent was evaporated and the residue dissolved on MeOH. The compound was purified by preparative HPLC (acidic system). The title compound was obtained in 6% yield (2.5 mg). MS (ESI+) calcd for C23H27N3O5S2: 489.139212. found 489.140522.

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, 13330-96-6, 4-(Dimethylamino)butan-1-ol.

Reference:
Patent; Martinsson, Jessica; Faernegardh, Katarina; Joensson, Mattias; Ringom, Rune; US2015/25068; (2015); A1;,
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Synthetic Route of 558-42-9, 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.558-42-9, name is 1-Chloro-2-methyl-2-propanol, molecular formula is C4H9ClO, molecular weight is 108.5667, as common compound, the synthetic route is as follows.

[00351j Step 1: methyl 3-chloro-4-(2-hydroxy-2-methylpropoxy)benzoate [00352j A 500 ml 3 neck RB flask was fitted with a mechanical stirrer,a J-Kem temperature probe/controller, an addition funnel, a water cooled reflux condenser and a nitrogen inlet/outlet. The vessel was charged under a nitrogen atmosphere with methyl 3-chloro-4-hydroxy-benzoate (10 g, 53.6 mmol) and methylalcohol (40 ml) which provided a clear pale yellow solution. Stirring was commenced and the pot temperature was recorded at 19 °C. The vessel was then charged with potassium carbonate (30 g, 0.21 mol) added as a solid in one portion which resulted in an exotherm to 23 °C. Note: The potassium carbonate was ground to a fine powder prior to use. The resulting suspension was continued to stir at rt for 15 mm and thentreated with 1-chloro-2-methyl-propan-2-ol (11.6 g, 0.11 mol) added neat dropwise via addition funnel over 10 mm. The resulting reaction mixture/suspension was then heated to 70 °C and stirred for 20 h. The reaction mixture was cooled to rt and diluted with ethyl acetate (250 ml). The mixture was filtered through a glass fit Buchner funnel with a 10 mm layer of Celite. The filter cake was washed with ethyl acetate (2 x100 ml). The filtrate was transferred to a separatory funnel and partitioned with 1 M aqueous NaOH (250 ml). The organic was removed and washed with 1 M aqueous NaOH (2 x 150 ml), saturated aqueous sodium chloride (150 ml), dried over sodium sulfate (250 g) and filtered through a glass frit Buchner funnel. The filtrate was concentrated under reduced pressure to provide methyl 3-chloro-4-(2-hydroxy-2-methylpropoxy)benzoate (9.0 g, 65percent) as a clear pale yellow oil. The material was used without further purification in the next synthetic step. ESI-MS mlz caic. 258.7, found 259.2 (M+1) Retention time: 1.46 mm (3 mm run).

The chemical industry reduces the impact on the environment during synthesis 558-42-9, I believe this compound will play a more active role in future production and life.

Reference:
Patent; VERTEX PHARMACEUTICALS INCORPORATED; DENINNO, Michael, Paul; ANDERSON, Corey; CONROY, Erica, Lynn; FRIEMAN, Bryan, A.; GROOTHENHUIS, Peter, Diederik Jan; HADIDA-RUAH, Sara, Sabina; HURLEY, Dennis, James; PIERRE, Fabrice Jean, Denis; SILINA, Alina; UY, Johnny; ZHOU, Jinglan; WO2015/6280; (2015); A1;,
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Related Products of 37585-16-3, 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 37585-16-3, name is (2-Amino-4-chlorophenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows.

A suspension of (2-amino-4-chlorophenyl)methanol (5.9 g) in ethyl acetate (100 mL) was heated until the former dissolved. Acetic anhydride (8 mL) was added and the mixture removed from the heat. The precipitate was filtered to give a white solid and the filtrate was concentrated and slurried with hexane and filtered to give further white solid. The two batches were combined to give 5.3 g of the alcohol intermediate. The first phase of the experiment was repeated on 3x the scale described above. 21 g of the combined products was dissolved in DCM (650mL) and added to a solution of thionyl chloride (23 mL) in DCM (225 mL) at room temperature under argon. The mixture was stirred for 30 minutes and concentrated to give a yellow/red solid. The solid was dissolved in DCM (500 mL), washed with saturated sodium bicarbonate (200 mL) and dried over magnesium sulfate. Removal of the solvent gave the 22 g of the title compound as a yellow/brown solid.

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 37585-16-3, (2-Amino-4-chlorophenyl)methanol.

Reference:
Article; Smethurst, Chris A.; Bevan, Nicola; Emmons, Amanda; Mookherjee, Claudette; Moores, Kitty; Peace, Simon; Piercy, Val; Watson, Steve P.; Zippoli, Mara; Brooks, Carl; Gough, Peter J.; Philp, Joanne; Bioorganic and medicinal chemistry letters; vol. 22; 23; (2012); p. 7252 – 7255,4;; ; Article; Smethurst, Chris A.; Bevan, Nicola; Brooks, Carl; Emmons, Amanda; Gough, Peter J.; Mookherjee, Claudette; Moores, Kitty; Peace, Simon; Philp, Joanne; Piercy, Val; Watson, Steve P.; Zippoli, Mara; Bioorganic and Medicinal Chemistry Letters; vol. 22; 23; (2012); p. 7252 – 7255;,
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Electric Literature of 349-75-7, 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 349-75-7 as follows.

General procedure: An alcohol(2.25±6.1 equiv) was added dropwise to a cooled suspension of NaH (60% dispersion in mineraloil; 2.2±6 equiv) in dry THF (0.5±1.5 mL) at 0 C and the mixture was stirred for 1 hunder argon atmosphere. A solution of 10 in dry THF (0.5±1.5 mL) was added dropwise andmixture was stirred overnight letting to warm up to rt. The reaction was quenched with icewater and acidified with a solution of KHSO4 until pH3. The aqueous phase was extractedwith EtOAc. The combined organic layers were washed with brine and the solvent was evaporatedunder reduced pressure at 40 C. The crude residue was purified by flash column chromatographywith appropriate eluents and a gradient.Heptyl 6-(heptyloxy)-2-[(4-methoxyphenoxy)methyl]-5-methylpyrimidine-4-carboxylate(11). General procedure III was followed except that the mixture containing the alkoxidewas added dropwise to the solution of 10. NaH (60% in mineral oil; 69.2 mg, 1.73 mmol, 2.2equiv), dry THF (1.25 mL), 1-heptanol (0.250 mL, 1.77 mmol, 2.25 equiv); compound 10(0.300 g, 0.787 mmol), dry THF (1.25 mL). Flash chromatography eluents: cyclohexane (A),EtOAc (B); gradient: 10%30% B×15 CV. Compound 11 was isolated as an orange oil (46.6mg, 0.0958 mmol, 12.2% yield).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,349-75-7, its application will become more common.

Reference:
Article; Provenzani, Riccardo; Tarvainen, Ilari; Brandoli, Giulia; Lempinen, Antti; Artes, Sanna; Turku, Ainoleena; Jaentti, Maria Helena; Talman, Virpi; Yli-Kauhaluoma, Jari; Tuominen, Raimo K.; Boije af Gennaes, Gustav; PLoS ONE; vol. 13; 4; (2018);,
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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, SDS of cas: 111-46-6, blongs to alcohols-buliding-blocks compound. SDS of cas: 111-46-6

To a solution of 2,2′-oxodiethanol (19.7 mL, 206.7 mmol, 3.0 eq.) In anhydrous tetrahydrofuran (100 mL) was added sodium (0.1 g).Stir the mixture until the sodium mass disappears,Tert-butyl acrylate (10.0 mL, 68.9 mmol, 1.0 eq.) Was then added dropwise.The mixture was stirred overnight,Brine (200 mL) was added and extracted with ethyl acetate (3 x 100 mL). The organic layer was washed with brine (3 × 300 mL),Dried over anhydrous sodium sulfate, filtered,Concentrated and purified by silica gel column chromatography (1: 1 n-hexane / ethyl acetate),A colorless oil was obtained (8.10 g, 49.4% yield).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,111-46-6, 2,2′-Oxybis(ethan-1-ol), and friends who are interested can also refer to it.

Reference:
Patent; Hangzhou Duo Xi Biological Technology Co., Ltd.; Zhao Luoboyongxin; Huang Yuanyuan; Yang Qingliang; Gai Shun; Ye Hangbo; Xu Yifang; Guo Huihui; Cao Minjun; Li Wenjun; Cai Xiang; Zhou Xiaomai; Xie Hongsheng; Jia Junxiang; Guo Zhixiang; Lin Chen; Yang Yanlei; Ye Zhicang; Qi Tafamingrenqingqiubugongkaixingming; (338 pag.)CN110621673; (2019); A;,
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Reference of 53463-68-6, 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.53463-68-6, name is 10-Bromodecanol, molecular formula is C10H21BrO, molecular weight is 237.18, as common compound, the synthetic route is as follows.

10-Bromodecanol (50 g, 210 mmol) was oxidized using pyridiniumchlorochromate (90.5 g, 420 mmol) in CH2Cl2 (800 mL) at room temperature for 3 h. The organic layerwas filtered, and the residual was washed with petroleum. Removal of the solvent from the combinedorganic layers in vacuo gave a dark oil. The dark-colored residue was chromatographed over SiO2,and elution with hexane/EtOAc (30:1, v/v) gave crude 10-bromodecanal. Triethyl orthoformate (44.5g, 300 mmol) and p-sulphonic acid monohydrate (0.57 g, 3 mmol)were added to a stirred and ice-cooled solution of the crude 10-bromodecanal in anhydrous ethanol(300 mL). After the exothermic reaction had subsided, the mixture was left at 0 C overnight. Water wasthen added, and the mixture was made basic by adding K2CO3 solution. The mixture was extractedwith diethyl ether, and then washed with brine and dried over MgSO4. The solvent was removedunder reduced pressure and the product was chromatographed on silica (hexane/EtOAc (25:1, v/v)),which gave crude 1,l-diethoxy-10-bromodecanal.This product was converted into the title iodide by being stirred for 4 h with sodium iodide(90 g, 600 mmol) in dry acetone (500 mL) under reflux. The solvent was removed under reducedpressure, the mixture was diluted with water (200 mL), and the product was extracted withpetroleum. The extracts were washed with water, 1% Na2S2O3 solution, and brine; dried overNa2SO4; and concentrated under reduced pressure. The resulting residue was chromatographed overSiO2. Elution with hexane/EtOAc (25:1, v/v) was conducted to yield 1,l-diethoxy-10-iododecan (5) as anoil (58.8 g, 78% yield based on 10-bromodecanol); 1H-NMR (500 MHz, CDCl3) delta 1.21 (6H, t, J = 7.0 Hz),1.29 (12 H, m), 1.60 (2 H, m), 1.82 (2H, m), 3.19 (2H, t, J = 7.0 Hz), 3.49 (2H, m), 3.64 (2H, m), 4.48 (1H, t,J = 6.0 Hz); 13C-NMR (125 MHz, CDCl3) delta 102.9, 60.8, 60.8, 33.6, 33.5, 30.5, 29.4, 29.4, 29.3, 28.5, 24.7,13.4, 15.4, 7.3.

Statistics shows that 53463-68-6 is playing an increasingly important role. we look forward to future research findings about 10-Bromodecanol.

Reference:
Article; Liu, Fu; Kong, Xiangbo; Zhang, Sufang; Zhang, Zhen; Molecules; vol. 24; 9; (2019);,
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Adding a certain compound to certain chemical reactions, such as: 86770-74-3, 2-(2-(2-(2-Aminoethoxy)ethoxy)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, COA of Formula: C8H19NO4, blongs to alcohols-buliding-blocks compound. COA of Formula: C8H19NO4

A solution of 3 (100 mg, 0.116 mmol) in chlorobenzene (5.0 mL) was added to the mixture of 42 (67.4mg, 0.349 mmol) and triethylamine (35.3 mg, 0.349 mmol), and the mixture was stirred at roomtemperature. After18 h, the reaction mixture was evaporated to dryness. The residue was purified bycolumn chromatography (silica gel; CHCl3/MeOH = 25/1) and dried in vacuo to give 5 as a blackishsolid (24.1 mg, 23.8 %). Rf = 0.35 (CHCl3/MeOH, 10:1). 1H NMR (400 MHz, CDCl3, delta): 8.95 (s, -CH2NHCO-, 2H), 3.86-3.54 (m, HO-CH2CH2-, -CH2CH2NHCO-, 32H), 1.93 (br, HO-CH2CH2-, 2H),13C NMR (100 MHz, CDCl3): delta (ppm) = 163.0, 146.0, 145.3, 144.7, 144.4, 143.9, 143.1, 143.0, 142.4,142.3, 140.8, 138.0, 74.5, 72.7, 70.7, 70.5, 70.3, 70.1, 61.8, 59.8, 40.6. IR (KBr, cm-1): 3263, 2860,1653, 1543. UV (DMSO) lambdamax, nm (epsilon × 10-3, M-1cm-1): 265 (10), 330 (4.0).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,86770-74-3, 2-(2-(2-(2-Aminoethoxy)ethoxy)ethoxy)ethanol, and friends who are interested can also refer to it.

Reference:
Article; Narumi, Atsushi; Nakazawa, Tatsufumi; Shinohara, Kosuke; Kato, Hiroki; Iwaki, Yoshinori; Okimoto, Haruya; Kikuchi, Moriya; Kawaguchi, Seigou; Hino, Shodai; Ikeda, Atsushi; Shaykoon, Montaser Shaykoon Ahmed; Shen, Xiande; Duan, Qian; Kakuchi, Toyoji; Yasuhara, Kazuma; Nomoto, Akihiro; Mikata, Yuji; Yano, Shigenobu; Chemistry Letters; vol. 48; 10; (2019); p. 1209 – 1211;,
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Synthetic Route of 558-42-9, 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.558-42-9, name is 1-Chloro-2-methyl-2-propanol, molecular formula is C4H9ClO, molecular weight is 108.5667, as common compound, the synthetic route is as follows.

To a solution of ethyl 9′-hydroxy-1 0′-methyl-2′-oxo-2′,7′-dihydrospiro[cyclobutane-1 ,6′-pyrido[2, 1-a]isoquinoline]-3′-carboxylate (200 mg, 0.59 mmol)in DMF (3 ml) was added K2C03 (407.1 mg, 2.95 mmol), Nal (353.7 mg, 2.36 mmol), and1-chloro-2-methylpropan-2-ol (256.2 mg, 2.36 mmol). The reaction mixture was stirred at 90 oc for 2 h. Then the reaction was extracted with DCM twice, the combined organic phaseswere washed with brine, dried over Na2S04, filtered and concentrated. The residue waspurified by chromatography (silica gel, 0-40percent CH30H in DCM) to afford the title compound(106 mg, 43.7percent yield). LCMS (ESI) m/z: 412.4 (M + 1t.

Statistics shows that 558-42-9 is playing an increasingly important role. we look forward to future research findings about 1-Chloro-2-methyl-2-propanol.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; CATALANO, John G.; DICKSON, Hamilton D.; KAZMIERSKI, Wieslaw Mieczyslaw; LEIVERS, Martin R.; WEATHERHEAD, John Gordon; (389 pag.)WO2018/154466; (2018); A1;,
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