Tag: M.W=100-200

Synthetic Route of 34145-05-6 ,Some common heterocyclic compound, 34145-05-6, molecular formula is C7H6Cl2O, 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 96-a (1.00 g, 5.65 mmol, 1.00 eq) and CDI (2.75 g, 16.95 mmol, 3.00 eq) was dissolved in tetrahydrofuran (20 mL), and stirred at 20C for 1 hour. Compound 7-a (1.78 g, 11.30 mmol, 1.74 mL, 2.00 eq) and triethylamine (1.72 g, 16.95 mmol, 2.35 mL, 3.00 eq) were then added to the above solution, and stirred at 80C for another 15 hours. After the reaction was completed, the reaction solution was added with 100 mL of water, and separated. The aqueous phase was further extracted with dichloromethane (200 mL 3 2). The organic phases were combined, and washed with saturated sodium hydrogen carbonate solution (150 mL) and saturated brine (100 mL). The organic phase was dried over anhydrous sodium sulfate, filtered, concentrated, and separated by column chromatography (petroleum ether : ethyl acetate = 10:1?6:1) to give the product of compound 96-b (1.9 g, yield: 93%). 1HNMR (400MHz, CHLOROFORMd) delta= 7.38 (d, J=2.4Hz, 1H), 7.34-7.28 (m, 1H), 7.26-7.22 (m, 1H), 5.21 (br. s., 2H), 4.17 (q, J=7.2 Hz, 4H), 3.09-2.89 (m, 2H), 2.50 (s, 1H), 1.99-1.89 (m, 2H), 1.76-1.64 (m, 2H), 1.28 (t, J=7.1 Hz, 3H). LCMS m/z = 360.0 [M+H]+.

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. 34145-05-6, (2,5-Dichlorophenyl)methanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Chia Tai Tianqing Pharmaceutical Group Co., Ltd.; Medshine Discovery Inc.; HE, Haiying; WU, Songliang; LUO, Zhi; MOU, Jianfeng; GUO, Fengying; WANG, Chuan; LI, Guoqing; ZENG, Minggao; CHEN, Shuhui; (199 pag.)EP3456711; (2019); A1;,
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Electric Literature of 889884-94-0, 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. 889884-94-0, name is 7-Fluoronaphthalen-2-ol, molecular formula is C10H7FO, 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.

General procedure: To a stirred solution of naphthol 35 (100 mg, 0.57 mmol) and azido acetate 13 (300 mg, 1.15 mmol) and 4 A molecular sieves in methylene chloride (40 mL) was added tin(IV) chloride (3.5 mL,1Min DCM, 3.5 mmol) at -78 C. The reaction mixture was stirred at -78 C for 10 min and then the temperature was gradually increasedto -35 C and kept overnight. The reaction was quenched with saturated sodium sulfate and the mixture was extracted with methylene chloride. The organic phase was dried and concentrated and purified by flash column chromatography (using 20% EtOAc/hexanes as eluent) to obtain 39 (43 mg, 20%) as yellow semisolid.

According to the analysis of related databases, 889884-94-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Mitra, Prithiba; Mandal, Subhajit; Chakraborty, Soumen; Mal, Dipakranjan; Tetrahedron; vol. 71; 34; (2015); p. 5610 – 5619;,
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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 7397-62-8, name is Butyl 2-hydroxyacetate. This compound has unique chemical properties. The synthetic route is as follows. COA of Formula: C6H12O3

a1 n-Butyl (t-butyl-dimethyl-silanyloxy)-acetate n-Butyl glycolate (231 g; 1.75 mol) and imidazole (345.1 g; 5.07 mol) are placed together at 0 C. The suspension obtained was treated portionwise with t-butyldimethylchlorosilane (303 g; 2.01 mol) during 1.5 hours. After 20 hours at room temperature the reaction mixture was diluted with ether/n-hexane 1:1 (1 l) and suction filtered. The crystals were rinsed thoroughly with ether/n-hexane 1:1 (200 ml). The filtrate was washed in succession with water (2*700 ml) and saturated aqueous sodium chloride solution (500 ml), dried over magnesium sulphate and concentrated. The oil obtained was distilled over a Vigreux column (7.5 cm). Yield: 405 g (94%) as a colourless oil (b.p. 78 C./0.98 mmHg). IR (film): 1760, 1225, 1206, 1148, 838, 780 cm-1 MS (EI): (M+H)+ 247

With the rapid development of chemical substances, we look forward to future research findings about 7397-62-8.

Reference:
Patent; Hoffmann-La Roche Inc.; US5464617; (1995); A;,
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Synthetic Route of 5020-41-7, Adding some certain compound to certain chemical reactions, such as: 5020-41-7, name is 2-(3-Methoxyphenyl)ethanol,molecular formula is C9H12O2, 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 5020-41-7.

Preparation B 2-(3-Methoxyphenyl)ethylbromide 114.1 g (750 mmol) of 2-(3-methoxyphenyl)ethanol was dissolved in 500 mL of benzene and cooled to 0 C. 35.5 mL (375 mmol) of PBr3 was slowly added to the stirring reaction and the reactin then heated to reflux under a nitrogen atmosphere for three hours. The reaction was quenched by the addition of water and the organic layer separated. The aqueous layer was washed twice with benzene and all the benzene extracts were combined. The benzene extract was washed twice with brine, dried with Na2 SO4, and evaporated to an oil. The oil was distilled and the fraction at 115-124 C. a 4 mm Hg was taken. This yielded 131.7 g of the title compound as a clear oil. PMR: Consistent with the proposed structure. MS: m/e=214, 216 (M) FD EA: Calc: C, 50.26; H, 5.16 Fd: C, 50.22; H, 5.02 C9 H11 BrO

According to the analysis of related databases, 5020-41-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Eli Lilly and Company; US5952350; (1999); A;,
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Synthetic Route of 583-03-9, 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. 583-03-9, name is 1-Phenylpentan-1-ol, molecular formula is C11H16O, 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.

The typical reaction steps are as follows:1 mmol of the starting alcohol of the reactant column shown in Table 2,OH – Ni3In-LDH 14 mg,Mesitylene 5mL were added to the reactor,Into the oxygen,Atmospheric reaction,The reaction was stirred at 60 for a certain period of time.The solid catalyst was removed by filtration,Using gas chromatography internal standard method (chlorobenzene as internal standard) to analyze the content of liquid products,Calculate yield.

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 583-03-9, 1-Phenylpentan-1-ol.

Reference:
Patent; Changzhou University; Zhou Weiyou; Dai Xuan; He Mingyang; Sun Fuan; Pan Jiugao; (8 pag.)CN107176898; (2017); A;,
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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. 39895-56-2, name is (4-(Aminomethyl)phenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows. Application In Synthesis of (4-(Aminomethyl)phenyl)methanol

To a solution of (2R,5S,8R, 14S,17R,20S,21S,22S,E)-8-benzyl-20-((E)-but-2-en- 2-yl)-14-((R)-sec-butyl)-2-isobutyl-557510, 17,2 l,25-hexamethyl-3,6,9, 12,15, 18,26-heptaoxo- 1 , 19-dioxa-4,7, 10, 13, 16-pentaazacyclohexacos-24-en-22-yl (4-nitrophenyi) carbonate (5.0 mg, 5.044 muetaiotaomicron, 1.0 eq; Intermediate 1 from Example 1) in DCM (0.1 mL, 5.04 muetaiotaomicron) was added (4-(aminomethyl)phenyl)methanol (3.46 mg, 0.025 mrnol , 5.0 eq) and DIPEA (8.81 muEpsilon, 0.050 mrnol, 10.0 eq) and stirred overnight. The reaction was monitored by reverse phase HPLC. The reaction mixture was concentrated on the rotavap and the crude residue obtained was purified by reverse phase flash chromatography (acetonitrile with 0.1% formic acid/ H20 with 0.1 % formic acid) to afford (2R,5S,8R,14S,17R,20S,21S,22S,E)-8-benzyl-20-((E)-but- 2-en-2-yl)-14-((R)-sec-butyl)-2-isobutyl-557 0,17,21,25-hexamethyl-356,9, 12s 15,18526- heptaoxo- 1 , 19-dioxa~4,7, 10, 13,16-pentaazacyclohexacos~24-en~22-yl ( – (hydroxymethy])benzyl)carbamate (2.75 mg, 2.78 muetaiotaomicron, 55.1 %). Observed HRMS (ESI) m/z: 989.565 | M 1 11

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, 39895-56-2, (4-(Aminomethyl)phenyl)methanol.

Reference:
Patent; SIRENAS LLC; USUI, Ippei; LEE, Bryan, Junn; COHEN, Steven, Bruce; MACHERLA, Venkat, Rami Reddy; BEVERAGE, Jacob, Neal; PAN, Chung-mao; BARMARE, Farhana; ESQUENAZI, Eduardo; (265 pag.)WO2018/45245; (2018); A1;,
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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.14002-80-3, name is Methyl 3-hydroxy-2,2-dimethylpropanoate, molecular formula is C6H12O3, molecular weight is 132.16, as common compound, the synthetic route is as follows.HPLC of Formula: C6H12O3

Example 2S nthesis of 2 , 2-dimethyl-3- (nitrooxy) propanoic acid HNO3 (2.4 mL, 54 mmol) was dissolved in AC2O (7.5 mL, 80 mmol) , cooled to 0C, and methyl 3-hydroxy-2 , 2-dimethylpropanoate (4 mL, 31 mmol) was added. The mixture was stirred for 1 hour, then poured into iced aHC03 (5%) and diluted with EtOAc. The organic phase was washed with brine, dried over Na2 S C>4 and concentrated affording methyl 2 , 2-dimethyl-3- (nitrooxy) propanoate as a clear oilThe residue was dissolved in NaOH (2.5 M, 20 mL) and MeOH (20 mL) and the solution was stirred at room temperature for 6 hours, and then acidified with HC1 (5%) to pH 3-4. The aqueous phase was extracted with EtOAc and the combined organic phases were washed with brine, dried over Na2 S C>4 and concentrated affording the title compound as a pale yellow solid (5.00 g, 98%)1H-NMR (CDCI3) : 4.53 (2H,s); 1.34 (6H,s).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,14002-80-3, Methyl 3-hydroxy-2,2-dimethylpropanoate, and friends who are interested can also refer to it.

Reference:
Patent; NICOX S.A.; ALMIRANTE, Nicoletta; IMPAGNATIELLO, Francesco; NICOTRA, Alessia; MANDELLI, Valentino; BRAMBILLA, stefania; WO2011/101245; (2011); A1;,
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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.1777-82-8, name is (2,4-Dichlorophenyl)methanol, molecular formula is C7H6Cl2O, molecular weight is 177.03, as common compound, the synthetic route is as follows.Product Details of 1777-82-8

General procedure: In a 50ml Pyrex round-bottom flask, a mixture of alcohol (1mmol), TBATB (10-20mg, 0.02-0.04mmol) in 10ml of CH3CN was exposed to blue or violet light LED irradiation at room temperature under an air atmosphere with stirring. The progress of the photocatalytic oxidation reaction was monitored by TLC on silica gel plates. The reaction mixture externally irradiated until the alcohol was completely consumed.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,1777-82-8, (2,4-Dichlorophenyl)methanol, and friends who are interested can also refer to it.

Reference:
Article; Mardani, Atefeh; Heshami, Marouf; Shariati, Yadollah; Kazemi, Foad; Abdollahi Kakroudi, Mazaher; Kaboudin, Babak; Journal of Photochemistry and Photobiology A: Chemistry; vol. 389; (2020);,
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Application of 19064-18-7, 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.19064-18-7, name is (2,6-Difluorophenyl)methanol, molecular formula is C7H6F2O, molecular weight is 144.12, as common compound, the synthetic route is as follows.

4.86 g of potassium tert-butoxide (43.3 mmol, 3.0 eq.) were added to a solution of 2.71 g of (2,6-difluorophenyl)methanol [CAS No.: 19064-18-7] (18.8 mmol, 1.3 eq.) in 120 ml of 1,2-dimethoxyethane, and the mixture was stirred at RT for 60 min. 2.60 g of 2-amino-3-chloro-5-methylpyrazine hydrochloride [CAS No.: 89182-14-9] (14.4 mmol, 1.0 eq.) were then added, and the mixture was stirred at 80 C. overnight. After cooling to room temperature, saturated aqueous sodium bicarbonate solution was added and the aqueous phase was extracted three times with dichloromethane. The combined organic phases were washed with saturated aqueous sodium chloride solution, dried with magnesium sulfate, filtered and concentrated. The residue was purified by Biotage Isolera (340 g silica gel cartridge, cyclohexane/ethyl acetate gradient, 10%-72% ethyl acetate). This gave 1.77 g of the title compound (39% of theory, purity 85%). (0262) LC-MS (Method 2): Rt=0.94 min (0263) MS (ESpos): m/z=252 (M+H)+ (0264) 1H-NMR (400 MHz. DMSO-d6): delta [ppm]=2.20 (s, 3H), 5.35 (s, 2H), 5.88 (s, 2H), 7.09-7.23 (m, 2H), 7.37 (s, 1H), 7.46-7.57 (m, 1H).

Statistics shows that 19064-18-7 is playing an increasingly important role. we look forward to future research findings about (2,6-Difluorophenyl)methanol.

Reference:
Patent; Bayer Pharma Aktiengesellschaft; VAKALOPOULOS, Alexandros; BROCKSCHNIEDER, Damian; WUNDER, Frank; STASCH, Johannes-Peter; MARQUARDT, Tobias; DIETZ, Lisa; LI, Min Jian Volkhart; (30 pag.)US2018/22751; (2018); A1;,
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Electric Literature of 702-98-7, Adding some certain compound to certain chemical reactions, such as: 702-98-7, name is 2-Methyladamantan-2-ol,molecular formula is C11H18O, 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 702-98-7.

To a stirred mixture of 2-methyl-2-adamantanol 14 (200 mg, 1.21 mmol), triethylamine(243 mg, 2.41 mmol) and acetic anhydride (246 mg, 2.41 mmol), 4-dimethylaminopyridine (DMAP) (18 mg, 0.12 mmol) was added as the acetylation catalyst. The mixture was stirred at room temperature for 72 h (TLC minitoring,hexane/ether 3:1). Petroleum ether was added and the mixture was washed withHCl 5%, saturated NaHCO3, brine and dried (Na2SO4). After solvent evaporation the residue was chromatographed on silica gel column using hexane-ether 4:1 as eluent to afford 150 mg (60 %) of pure acetyl derivative 20 (a second fraction including 2-methylene adamantane was obtained).

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. 702-98-7, 2-Methyladamantan-2-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Kolocouris, Antonios; Koch, Andreas; Kleinpeter, Erich; Stylianakis, Ioannis; Tetrahedron; vol. 71; 16; (2015); p. 2463 – 2481;,
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