Month: March 2021

Reference of 2425-41-4, 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. 2425-41-4, name is (2-Phenyl-1,3-dioxane-5,5-diyl)dimethanol, molecular formula is C12H16O4, 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.

To a solution of 5109 (1 0.0 g, 44.6 mmol) in dichloromethane (180 ml) under argon were addedbromoacetonitrile (13.0 g, 108.4 mmol), Silver( I) oxide (20.7 g, 89.2 mmol), and tetrabutylammonium iodide (3.3 g, 8.92 mmol), and the resulting mixture was stirred overnight. The mixture was filtered overCelite, and the filtrate was evaporated to give a black residue, which was subjected to flash silica gelcolumn purification on ISCO companion (hexane/ethyl acetate, 15 – 90%) to give 5.55 g (41 %) of thedesired compound S127 as a viscous oil. ESI MS for C15H1sN204 calculated 302.3, observed [M+H]+ 303.3.

According to the analysis of related databases, 2425-41-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SOLSTICE BIOLOGICS, LTD.; SAKAMURI, Sukumar; BRADSHAW, Curt, W.; ELTEPU, Laxman; MEADE, Bryan, R.; LAM, Son; (237 pag.)WO2018/35380; (2018); A1;,
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Reference of 7397-62-8, 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 7397-62-8 as follows.

Example 36 Butyl 3-amino-6-benzyl-5,6,7,8-tetrahydro-4H-furo[2,3-d]azepine-2-carboxylate A solution of 1.0 gm (0.008 mol) of butyl glycolate in 8 ml of absolute dioxane was added dropwise to a suspension of 0.4 gm (0.008 mol) of 50% sodium hydride in 5 ml of absolute dioxane, and the mixture was stirred for one hour at room temperature. Then, while the mixture was cooled with ice, a solution of 1.0 gm (0.004 mol) of 1-benzyl-4-chloro-5-cyano-2,3,6,7-tetrahydro-1H-azepine in 15 ml of absolute dioxane was added, and the mixture was stirred for one hour. The reaction mixture was then poured into about 80 ml of ice-cold water, and the aqueous mixture was extracted three times with ethyl acetate. The combined organic phases were washed twice with water, dried over sodium sulfate and concentrated by evaporation. The residue was purified by column chromatography on silicagel, using toluene/ethyl acetate (7:3) as eluant. Yield: 0.2 gm (14% of theory). Melting point: <20 C. Calc.: molecular peak m/e=342. Found: molecular peak m/e=342. These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,7397-62-8, its application will become more common. Reference:
Patent; Dr. Karl Thomae Gesellschaft mit beschrankter Haftung; US4414225; (1983); A;,
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Adding a certain compound to certain chemical reactions, such as: 42042-68-2, 4-(Methylamino)butan-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, Recommanded Product: 4-(Methylamino)butan-1-ol, blongs to alcohols-buliding-blocks compound. Recommanded Product: 4-(Methylamino)butan-1-ol

To a solution of 3.00 g of 2-chloro-5,6-di-p-tolylpyrazine and 1.57 g of 4-(methylamino)-1-butanol in 15 ml of N,N-dimethylformamide, 2.26 g of potassium carbonate was added.. After heating with stirring at 100C for 26 hours, the reaction solution was extracted with diethyl ether after adding ice water.. The extract was washed in turn with water and saturated brine and dried over anhydrous magnesium sulfate, and then the solvent was evaporated under reduced pressure.. The residue was purified by silica gel column chromatography and the resulting crystal was washed with diisopropyl ether to obtain 2.76 g of the desired compound as a colorless crystal having a melting point of 94 to 96C.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,42042-68-2, 4-(Methylamino)butan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; Nippon Shinyaku Co., Ltd.; EP1400518; (2004); A1;,
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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. 100-37-8, name is 2-(Diethylamino)ethanol. A new synthetic method of this compound is introduced below., name: 2-(Diethylamino)ethanol

Into a 250 ml four-necked flask equipped with a stirrer and a water separator and a reflux device were placed 12.8 g (0.1 mol) of adipic anhydride, 35.1 g (0.3 mol) of N, N-diethylaminoethanol,0.8gTitanyl sulfate, 20 mlXylene, stirring heated to 145 C refluxing reaction 3h, until the separation of 1.8g (0.1mol) water, remove the catalyst filter (direct reuse), the filtrate into another 250ml three bottles, vacuum distillation of solvent ), An excess amount of diethylaminoethanol (used for recovery), and a low boiling point substance were added, and 3.0 g of activated clay was added thereto. The mixture was stirred for 30 minutes, and the temperature was lowered to 80 C or less, and filtered to obtain a yellow oily liquid bisdiethylaminoethyl adipate 31.34 G, and the yield was 91.1%. And then adipic acid bis diethylamino ethanol ester and two times the citric acid mixed heated to 120 C, the citric acid after melting, stirring cooling crystallization salt, that is a white powder solid product adipic acid bis Diethylamino ethanolate citrate. Its melting point: 117 C.

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, 100-37-8, 2-(Diethylamino)ethanol.

Reference:
Patent; Suzhou Institute of Science and Technology; Wang, Yanlin; Wang, Hao; Wang, Siyuan; Qiu, Yexian; (13 pag.)CN105801441; (2016); A;,
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Synthetic Route of 2077-19-2, 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. 2077-19-2, name is 2-(4-Bromophenyl)propan-2-ol. A new synthetic method of this compound is introduced below.

1.1 4-[4-(1-Hydroxy-1-methyl-ethyl)-benzoyl]-piperidine-1-carboxylic acid tert- butyl ester To a solution of 2-(4-bromo-phenyl)-propan-2-ol (5.00 g; 22.78 mmol) in THF (100 mL) under nitrogen atmosphere, n-butyl lithium (23 % in hexanes) (13.92 ml; 50.12 mmol) was added dropwise at -78 C and stirred for 15 min at the same temperature. A solution of 4-(methoxy-methyl-carbamoyl)-piperidine-1- carboxylic acid tert-butyl ester (6.96 g; 25.06 mmol) in THF ( 00 mL) was added dropwise at -78 C and stirred for 2 h at -78 C. The reaction mixture was stirred for 4 h at -78 C and quenched with saturated NH4CI solution (100 mL). The reaction mixture was extracted with ethyl acetate (2 x 100 mL). The combined extracts were washed with water (200 mL), brine solution (100 mL), dried over anhydrous sodium sulfate and concentrated. The residue was purified by column chromatography using silica gel (60-120) and petrol ether – ethyl acetate (1 :1) as gradient elution to afford the title compound (2.30 g; 29 %) as a pale yellow oil; H NMR (400 MHz, CDCI3) delta 7.92 (d, J = 8.48 Hz, 2H), 7.60 (d, J = 8.52 Hz, 2H), 5.18 (s, 1 H), 3.96 (d, J = 12.56 Hz, 2H), 3.63-3.57 (m, 1 H), 2.90 (s, 2H), 1.74 (d, J = 11.52 Hz, 2H), 1.43-1.38 (m, 17H); LC/MS (B), Rt: 4.50 min; (M+H-BOC) 248.3.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2077-19-2, 2-(4-Bromophenyl)propan-2-ol, and friends who are interested can also refer to it.

Reference:
Patent; MERCK PATENT GMBH; DORSCH, Dieter; BUCHSTALLER, Hans-Peter; WO2015/14442; (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 124-68-5, name is 2-Amino-2-methyl-1-propanol. This compound has unique chemical properties. The synthetic route is as follows. Recommanded Product: 124-68-5

General procedure: A microwave tube was charged with 2i (1 mmol), NaOH (120 mg, 3 mmol), and EtOH (10 mL). The tube was sealed, placed in a microwaveoven and heated (T = 135 C; t = 10 min). After release, Boc2O(655 mg, 3 mmol) was added at r.t. and the reaction mixture wasstirred for 2 h at 40 C. H2O (10 mL) and Et2O (20 mL) were added andthe layers were separated. The aqueous phase was extracted withEt2O (2 ¡Á 20 mL) and the combined organic layers were dried overMgSO4, filtered, and the solvent was removed in vacuo. The crude residuewas purified on silica gel chromatography (cyclohexane-EtOAc,95:5 to 40:60) to afford the desired N-Boc-protected amino alcohol 4.

With the rapid development of chemical substances, we look forward to future research findings about 124-68-5.

Reference:
Article; Boukattaya, Fatma; Caille, Julien; Ammar, Houcine; Rouzier, Florian; Boeda, Fabien; Pearson-Long, Morwenna S. M.; Bertus, Philippe; Synthesis; vol. 48; 6; (2016); p. 906 – 916;,
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Adding a certain compound to certain chemical reactions, such as: 6850-39-1, 3-Aminocyclohexanol, 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, name: 3-Aminocyclohexanol, blongs to alcohols-buliding-blocks compound. name: 3-Aminocyclohexanol

To a solution of 4-chloropyrrolo[l,2-b]pyridazine-3-carbonitrile (15g) (0.15 g, 0.84 mmol) in DMF (2.5 mL) was added at room temperature 3-aminocyclohexanol (5In) (194 mgs, 1.68 mmol), DIPEA (0.87 mL, 5 mmol) and stirred at room temperature overnight. The reaction was quenched with water (10 mL) and extracted with ethyl acetate (10 mL). The aqueous layer was separated and extracted with ethyl acetate (2 x 10 mL). The organic layers were combined washed with water (2 x 10 ml), brine (10 mL), dried, filtered and concentrated in vacuum. The residue obtained was purified by flash column chromatography (silica gel 12g, eluting with 0- 100% ethyl acetate in hexanes) to furnish 4-(3-hydroxycyclohexylamino)pyrrolo[l,2- b]pyridazine-3-carbonitrile (51o) (0.105 g, 46 %) as a white solid: 1H NMR (300 MHz, DMSO) delta 7.90 (s, IH), 7.78 (d, J= 8.5 Hz, IH), 7.69 (dd, J= 2.6, 1.6 Hz, IH), 7.12 (dd, J= 4.4, 1.6 Hz, IH), 6.68 (dd, J= 4.4, 2.7 Hz, IH), 4.88 (d, J= 4.3 Hz, IH), 4.25 (m, IH), 3.54 (m, IH), 2.17 (m, IH), 1.92 (m,lH), 1.76 (d, J= 13.3 Hz, 2H), 1.54 – 1.24 (m, 3H), 1.16 (dd, J= 14.6, 10.6 Hz, IH). MS (ES+) 536.3 (2M+Na), MS (ES-) 291.0 (M+Cl).

The synthetic route of 6850-39-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BIOCRYST PHARMACEUTICALS, INC.; BABU, Yarlagadda S.; KOTIAN, Pravin L.; KUMAR, V. Satish; WU, Minwan; LIN, Tsu-Hsing; WO2011/14817; (2011); 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 37585-16-3, name is (2-Amino-4-chlorophenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows. Recommanded Product: (2-Amino-4-chlorophenyl)methanol

(2-amino-4-chlorophenyl) methanol (6. 6g, 0. 04mol), 1-(3, 5-dimethylphenyl) ethanone(10. 0g, 0. 068mol), RuCl 2 (PPh 3) 3 (0. 1g), and 2. 4g of a KOH, 100 ml of toluene and 10 is made to circulate at a time. By using a dien-stark trap, the collected water from the reaction. After cooling to room temperature, the reaction, the mixture is filtered through a silica gel plug. The product, further purified by using column chromatography eluent ethyl acetate Phenylbicyclohexane 2%. After the column, 9g of the product is obtained. Furthermore, this product is recrystallized from isopropanol. 5g of the desired product is obtained.

With the rapid development of chemical substances, we look forward to future research findings about 37585-16-3.

Reference:
Patent; UNIVERSAL DISPLAY CORPORATION; ALLEYNE, BERT; KWONG, RAYMOND; YEAGER, WALTER; XIA, CHUANJUN; (72 pag.)JP2015/212297; (2015); A;,
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Electric Literature of 3068-00-6, 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. 3068-00-6, name is 1,2,4-Butanetriol, molecular formula is C4H10O3, 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 solution of CoCl2 (0.6 mmol) in anhyd MeCN (4 mL), the selecteddialkyl acetal (1 mmol), TMSCl (1.1 mmol), and butane-1,2,4-triol (3 mmol) were added, with stirring, at r.t. At the end ofthe reaction, the mixture was extracted with EtOAc and the combinedextracts were washed with 5% NaHCO3. The organic layerwas dried (anhyd Na2SO4) and filtered, and the solvent was evaporatedunder vacuum. The oils obtained were purified by flash chromatographyto give the desired compounds.

According to the analysis of related databases, 3068-00-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Battisti, Umberto Maria; Sorbi, Claudia; Franchini, Silvia; Tait, Annalisa; Brasili, Livio; Synthesis; vol. 46; 7; (2014); p. 943 – 946;,
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Reference of 112513-79-8, 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.112513-79-8, name is 6,7-Dihydro-5H-pyrrolo[1,2-a]imidazol-7-ol, molecular formula is C6H8N2O, molecular weight is 124.1405, as common compound, the synthetic route is as follows.

To a mixture of 6,7-dihydro-5H- pyrrolofl,2-a]imidazol-7-ol (1 g, 8.06 mmol) and 3-methyl-4-nitro-lH-pyrazole (1.13 g, 8.87 mmol) in THF (20 mL) was added PPh3 (3.17 g, 12.09 mmol) and then D1AD (2.44 g, 12.09 mmol, 2.4mL) dropwise at 0 C over a period of 30 min under N2. The mixture was warmed to 20 C and stirred for 12 h, then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (gradient PE:EtOAc from 10: 1 to 0: 1) to give the mixture of 7-(3-methyl-4-nitro-pyrazol-l-yl)-6,7-dihydro-5H-pyrrolo[l,2-a]imidazole and 7-(5-methyl- 4-nitro-lH-pyrazol-l -yl)-6,7-dihydro-5H-pyrrolo[l,2-a]imidazole as a white solid. LCMS: RT 0.112 min, m/z —— 234.1 [M + H .] To a solution of 7-(3- methyl-4-nitro-pyrazol-l-yl)-6,7-dihydro-5H-pyrrolo| l,2-a|imidazole and 7-(5-methyl-4-nitro-lH- pyrazol-l-yl)-6,7-dih}’dro-5H-pyrrolo[ l,2-a]imidazole (650 mg, 2.79 mmol) in MeOH (20 mL) was added Pd-C (10%, 0.3 g) under N2. The suspension was degassed under vacuum and purged with H2 several times. The mixture was stirred under H2 (15 psi) at 20 C for 4 h, then filteredand concentrated under reduced pressure, to give the mixture of l-(6,7-dihydro-5H-pyrrolo|T,2- a]imidazol-7-yl)-3-methyl-pyrazol-4-amine and l-(6,7-dihydro-5H-pyrrolo[ l,2-a]imidazol-7-yl)-5- methyl-lH-pyrazol-4-amine as a light yellow solid. LCMS: RT 0.62-0.878 min, m/z = 204.2 [M+H]~.

Statistics shows that 112513-79-8 is playing an increasingly important role. we look forward to future research findings about 6,7-Dihydro-5H-pyrrolo[1,2-a]imidazol-7-ol.

Reference:
Patent; DENALI THERAPEUTICS INC.; ESTRADA, Anthony A.; FENG, Jianwen A.; LYSSIKATOS, Joseph P.; SWEENEY, Zachary K.; DE VICENTE FIDALGO, Javier; (271 pag.)WO2017/87905; (2017); A1;,
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