Category: alcohols-buliding-blocks

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 558-42-9, name is 1-Chloro-2-methyl-2-propanol. This compound has unique chemical properties. The synthetic route is as follows. name: 1-Chloro-2-methyl-2-propanol

[00302j 5-(2-fluoro-2-methyl-propoxy)-6-methoxy-pyridine-2- carboxylic acid [00303j A mixture of 1-chloro-2-methyl-propan-2-ol (10 mL, ), 4- hydroxy-3-methyl-benzoic acid (2.0 g, 13.2 mmol), K2C03 (7.3 g, 52.7 mmol), H20 (6.0 mL) and ethanol (60 mL) was heated at 80 °C overnight. The reaction mixturewas cooled to rt, partitioned between iN NaOH and EtOAc and the layers separated. The organic layer was washed with iN NaOH (2x) and the combined aqueous layers were washed with EtOAc. The combined organics were concentrated under reduced pressure and diluted with EtOH (15 mL). The mixture was treated with H20 (2 mL) and NaOH (1.0 g, 26.3 mmol). The reaction mixture was stirred at 40 °C for 4 h. Thereaction mixture was poured into iN NaOH and extracted with ether (2x). The pH was brought to 2-3 with 6N HC1 and the aqueous material was extracted with EtOAc (3x). The organics were combined, washed with saturated aqueous NaC1, dried (Na2SO4), filtered, and evaporated to dryness. The material was triturated with ether to provide 4-(2-hydroxy-2-methyl-propoxy)-3-methyl-benzoic acid (2.2 g, 75percent) as a white solid.?H NMR (400 MHz, DMSO) d 7.75 (dd, J = 8.5, 2.0 Hz, 1H), 7.73 – 7.70 (m, 1H), 6.96 (d, J = 8.6 Hz, 1H), 4.67 (s, 1H, OH), 3.76 (s, 2H), 2.20 (s, 3H), 1.22 (s, 6H). ESI-MS mlz calc. 224.1, found 225.5 (M+1) Retention time: 1.06 mm (3 mm run).

With the rapid development of chemical substances, we look forward to future research findings about 558-42-9.

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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Application of 3973-18-0, 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. 3973-18-0, name is Propynol ethoxylate, molecular formula is C5H8O2, 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.

[Synthesis 7]Production of 2-((4-methylcyclohexa- l,4-dienyl)methoxy)ethyl4-methylbenzenesulfonate and 2-((5-methylcyclohexa- l,4-dienyl)methoxy)ethyl 4-methylbenzenesulfonate (1,4type) (1,4type)+ +In 400 ml of toluene, 100.00 g (0.59 mol) of the diene alcohols obtained in Synthesis 6, 90.29 g (0.89 mol) of triethylamine, 73.20 g (0.89 mol) of 1-methylimidazole were dissolved. To this solution cooled in an ice bath, a toluene solution (400 ml) of 130.33 g (0.68 mol) of p-toluenesulfonyl chloride was added dropwise slowly, followed by stirring at room temperature for 1 hour. Water was added thereto, and phase separation was conducted. The obtained organic layer was washed with 15% sulfuric acid, water, and saturated aqueous sodium hydrogen carbonate in this order. The solvent was removed by distillation under reduced pressure. Thus, 188.01 g of the target tosylates were obtained as a colorless oily substance. Yield: 98.1% (l,4-type/l,5-type=91/9). ?-NMR (CDC13, 300 MHz) ?:1.67 (s, 3H), 2.44 (s, 3H), 2.58 (brs, 4H), 3.58-3.55 (m, 2H), 3.84 (s, 2H), 4.18-4.14 (m, 2H), 5.41-5.40 (m, 1H), 5.64-5.63 (m, 1H), 7.33 (d, J=8.3 Hz, 1H), 7.80 (d, J=8.3 Hz, 1H);HRMS (ESI):[M+H]+ calcd for C17H22O4S: 323.1312; found: 323.1325

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 3973-18-0, Propynol ethoxylate.

Reference:
Patent; TAKASAGO INTERNATIONAL CORPORATION; TANAKA, Shigeru; TOUGE, Taichiro; NARA, Hideki; ISHIDA, Kenya; WO2013/65867; (2013); A1;,
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Reference of 722-92-9, 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 722-92-9, name is 2-(4-Aminophenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol. This compound has unique chemical properties. The synthetic route is as follows.

General procedure: To a solution of 12a-e in DMSO (500 L) were added 4-(hexafluoro-2-hydroxyisopropyl)aniline (2 eq.)and N,N-diisopropylethylamine (2 eq.) at room temperature. The mixture was stirred for 15 min at 100 C,then poured into dilute hydrochloric acid and extracted with EtOAc. The organic layer washed with brine,dried over sodium sulfate and concentrated. The residue was purified by recrystallization from MeOH.

According to the analysis of related databases, 722-92-9, the application of this compound in the production field has become more and more popular.

Reference:
Article; Kaitoh, Kazuma; Toyama, Hirozumi; Hashimoto, Yuichi; Fujii, Shinya; Heterocycles; vol. 95; 1; (2017); p. 547 – 556;,
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Synthetic Route of 41175-50-2 ,Some common heterocyclic compound, 41175-50-2, molecular formula is C12H15NO, 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.

Compound 26 (0.13 g, 0.69 mmol) was dissolved in 1 mL MeOH. The solution was chilled in an ice bath, then was treated with HC1 (2 M, 10 mL). After 15 mins, />-nitrobenzenediazonium tetrafluoroborate (0.18 g, 0.76 mmol) was added to the solution in 5 portions over 15 mins, then stirred at 0 C for additional 1 h. During which time, the color of the reaction mixture changed from orange to dark red. After which, the solution was carefully basified with solid K2CO3 until pH value of the solution rose above 8. The deep red precipitate was collected via vacuum filtration and washed with small portions of DI water. The product was left in the funnel and air dried overnight to afford compound 36 (186 mg, 80%) as a dark red solid, which was used for the next step without further purification.

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. 41175-50-2, 1,2,3,5,6,7-Hexahydropyrido[3,2,1-ij]quinolin-8-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; OREGON HEALTH & SCIENCE UNIVERSITY; GIBBS, Summer L.; WANG, Lei G.; BARTH, Connor W.; (159 pag.)WO2020/23911; (2020); A2;,
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Adding a certain compound to certain chemical reactions, such as: 1124-63-6, 3-Cyclohexylpropan-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, category: alcohols-buliding-blocks, blongs to alcohols-buliding-blocks compound. category: alcohols-buliding-blocks

3-Cyclohexylpropan-1-ol (10 mmol) was refluxed overnight with bromic acid (10 mmol). After adding ice water,The reaction mixture was extracted with ethyl acetate to give 3- (bromopropyl) cyclohexane. The crude mixture was reacted with phthalimide (15 mmol) in THF solution (20 ml) to obtain a white solid phthalimide derivative. This was filtered and then reacted with hydrazine (98%, 63 mmol) in anhydrous ethanol (15 ml) at 60 C for 10 minutes. The reaction mixture was diluted with water and extracted with ethyl acetate to give a 3-cyclohexylpropylamine compound.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,1124-63-6, 3-Cyclohexylpropan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; The Industry & Academic Cooperation in Chungnam National University (IAC); Jung, Sang-Hun; Woo, Sun-Hee; Kim, Sang- Kyum; Jeon, Eun-Seok; Lee, Yu-Jung; Meunikam, Manoj; Jalani, Hiteshkumar; Sharma, Niti; (205 pag.)KR2016/108281; (2016); A;,
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Reference of 14426-20-1 ,Some common heterocyclic compound, 14426-20-1, molecular formula is C6H16ClNO, 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.

Chenodeoxycholic acid (2.0 g, 5.1 mmol), DMAP (0.92 g, 7.6 mmol) and diethylaminoethanol hydrochloride (1.17 g, 7.6 mmol) were mixed and dissolved in dichloromethane (15 mL). ), EDCI (1.46 g, 7.6 mmol) was added in portions. After stirring at room temperature for 3 hours, water and dichloromethane were added and extracted three times. The organic phase was washed twice with saturated ammonium chloride and washed with saturated brine.Dry Na2SO4, concentrate by filtration,After column chromatography, chenodeoxycholic acid 2-(diethylamino)ethyl ester (2.99 g, 80%) was obtained.2-(Diethylamino)ethyl chenodeoxycholate (2.0 g, 4.1 mmol) was dissolved in 10 mL of glacial acetic acid, heated to 50 C for 2 hours, and glacial acetic acid was concentrated to obtain chenodeoxycholic acid 2 -(Diethylamino)ethyl acetate (2.24 g, 100%).

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. 14426-20-1, 2-(Diethylamino)ethanol hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Ningbo Bai Naxi Pharmaceutical Co., Ltd.; Li Xiaochuan; (20 pag.)CN108218945; (2018); A;,
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Adding a certain compound to certain chemical reactions, such as: 67622-86-0, 2-Methyl-1-(methylamino)propan-2-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, Application In Synthesis of 2-Methyl-1-(methylamino)propan-2-ol, blongs to alcohols-buliding-blocks compound. Application In Synthesis of 2-Methyl-1-(methylamino)propan-2-ol

To a suspension of l-methyl-4-nitro-lH-pyrazole-3-carboxylic acid (639 mg, 3.7 mmol) and 2- methyl-l-(methylamino)propan-2-ol (500 mg, 4.85 mmol) in THF (15 mL) were added HATU (1.57 g, 4.12 mmol) and N-methylmorpholine (2.13 mL, 19.4 mmol) at ambient temperature. The mixture was heated to 70 C and stirred for 16 h. After cooling down to ambient temperature, the reaction mixture was poured into 20 mL HC1 (2N aqueous solution) and extracted with ethyl acetate (2 x 100 mL).The organic layers were washed with water, brine and the solvent was evaporated. The aqueous layer was back-extracted with dichloromethane, dried and concentrated in vacuo. Both residues were combined to give 2.75 g of a semi-solid yellow material. The crude material was purified by silica gel chromatography using a methanol/ethyl acetate gradient to yield the product (1.2 g, 90 %) as colorless oil.MS: M = 257.3 (M+H)+

At the same time, in my other blogs, there are other synthetic methods of this type of compound,67622-86-0, 2-Methyl-1-(methylamino)propan-2-ol, and friends who are interested can also refer to it.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; BLEICHER, Konrad; FLOHR, Alexander; GROEBKE ZBINDEN, Katrin; GRUBER, Felix; KOERNER, Matthias; KUHN, Bernd; PETERS, Jens-Uwe; RODRIGUEZ SARMIENTO, Rosa Maria; WO2011/154327; (2011); A1;,
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Related Products of 3840-31-1, 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 3840-31-1 as follows.

A solution of alcohol 30?22 (396 mg, 2 mmol), imidazole (300 mg, 4.4mmol), and TBSCl (332 mg, 2.2 mmol) in anhyd CH2Cl2 (4 mL) was stirred at overnight at`1234/7458-+ * r.t. H2O (5 mL) and CH2Cl2 (20 mL) were addedto the mixture, and the organic layer was separated, washed successivelywith sat. aq NaHCO3 (5 mL), H2O (2 × 5 mL), and brine (5 mL),then dried (MgSO4) and filtered. The filtrate was concentrated in vacuoand the residue was purified by flash column chromatography [silicagel, EtOAc-PE (1:25)] to give a colorless oil; yield: 569 mg (91%).IR (KBr): 2962, 2928, 2857, 1596, 1499, 1459, 1378, 1017, 832, 775cm-1.1H NMR (300 MHz, CDCl3): delta = 6.57 (s, 2 H), 4.69 (s, 2 H), 3.85 (s, 6 H),3.83 (s, 3 H), 0.96 (s, 9 H), 0.11 (s, 6 H).13C NMR (75 MHz, CDCl3): delta = 153.16, 137.14, 136.78, 102.80, 64.86,60.78, 55.96, 25.89, 18.36, -5.28.MS (ESI, MeOH): m/z = 335 [M + Na]+.HRMS-ESI: m/z [M + Na]+ calcd for C16H28NaO4Si: 335.1655; found:335.1663.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,3840-31-1, its application will become more common.

Reference:
Article; Zhang, Qi; Kang, Xiuqin; Long, Lei; Zhu, Lijuan; Chai, Yonghai; Synthesis; vol. 47; 1; (2015); p. 55 – 64;,
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Electric Literature of 71176-54-0, 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. 71176-54-0, name is (5-Amino-1,3-phenylene)dimethanol, molecular formula is C8H11NO2, 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.

Compound 27:25 26 27[227] To a solution of 5-nitro-m-xylene-alpha,alpha’-diol 25 (1.07 g, 5.84 mmol) in methanol (50 mL) was added Pd/C (10percent, 311 mg, 0.29 mmol). Hydrogen was introduced to replace the air then the mixture was hydrogenated (H2, 5 psi) for 2 hours at room temperature. The solution was filtered through celite and the filtrate was evaporated by rotary evaporation in vacuo to give compound 26 as a white solid (900 mg, y = 100percent). 1H NMR (400 MHz, MeOD): delta 6.71 (s, IH), 6.66 (s, 2H), 4.51 (s, 4H); 13C NMR (400 MHz, MeOD): delta 148.9, 143.8, 116.7, 114.3, 65.5; It was dissolved in anhydrous acetonitrile (30 mL) and ethyl bromoacetate (443 mul, 4.67 mmol) and potassium carbonate (807 mg, 5.84 mmol) were added. The mixture was put in a 86 0C oil bath and refluxed for 17 hours. The reaction mixture was removed from the oil bath, cooled to room temperature and diluted with dichloromethane. It was filtered through celite and the solid was washed with dichloromethane. White precipitate appeared in the filtrate. It was col]ected by filtration to give compound 27 (414 mg, y = 39percent) as a white solid. 1H NMR (400 MHz, MeOD): delta 6.67 (s, IH), 6.53 (s, 2H), 4.51 (s, 4H), 3.94 (s, 2H), 3.73 (s, 3H); 13C NMR (400 MHz, MeOD): delta 174.0, 149.7, 143.9, 116.2, 111.6, 65.6, 52.6, 46.5; MS (m/z): found 248.0 (M + Na)+.

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 71176-54-0, (5-Amino-1,3-phenylene)dimethanol.

Reference:
Patent; IMMUNOGEN, INC.; LI, Wei; FISHKIN, Nathan, Elliott; ZHAO, Robert, Yongxin; MILLER, Michael, Louis; CHARI, Ravi, V., J.; WO2010/91150; (2010); A1;,
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Related Products of 112-27-6 ,Some common heterocyclic compound, 112-27-6, molecular formula is C6H14O4, 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.

Triethylene glycol (4.50 g, 30 mmol) and triethylamine (TEA) (8.0 mL) were dissolved in dichloromethane (60 mL). Then, tosylchloride (5.70 g, 30 mmol) was added in one portion. The resulting mixture was stirred for 12 h at 25 oC (Scheme 2). After washing with KHSO4 (1 mol/L, 40 mL) and NaHCO3 (5%, 40 mL) and drying over anhydrous Na2SO4, the crude product was obtained by evaporation and subsequently purified by column chromatography over silica gel (dichloromethane/MeOH = 100:1, v/v) to obtain the target product 1 as a colorless oil (4.2 g, 14.4 mmol, 48%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,112-27-6, its application will become more common.

Reference:
Article; Wu, Xuan; Gao, Lei; Sun, Junzhao; Hu, Xiao-Yu; Wang, Leyong; Chinese Chemical Letters; vol. 27; 11; (2016); p. 1655 – 1660;,
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