Month: July 2021

Synthetic Route of 2240-88-2, 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 2240-88-2, name is 3,3,3-Trifluoropropan-1-ol. This compound has unique chemical properties. The synthetic route is as follows.

Step 3; Preparation of tert-butyl 2-cvclopropyl-4-(3,3,3-trifluoropropoxy)-5,6,8,9- tetrahydro-7H-pyrimido[4,5-d]azepine-7-carboxylate; [057] 3,3,3-Trifluoropropan-1-ol (0.43 g, 3.7 mmol) was dissolved in 1 ,4-dioxane (5 mL). Potassium tert-butoxide (572 mg, 5.1 mmol) was added, and the mixture was stirred at rt for 15 min. tert-Butyl 4-chloro-2-cyclopropyl-5,6,8,9-tetrahydro-7H-pyrimido[4,5- EPO d]azepine-7-carboxylate (1.1 g, 3.4 mmol) was then added as a solution in 1 ,4-dioxane (5 ml_). The mixture was heated at 50°C overnight. The resulting white suspension was concentrated under reduced pressure, and the residue was partitioned between water and ethyl acetate. The organic layer was separated, dried (MgSO4), and concentrated under reduced pressure to give the title compound as a colorless oil (1.2 g, 94percent).

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 2240-88-2, 3,3,3-Trifluoropropan-1-ol.

Reference:
Patent; BAYER PHARMACEUTICALS CORPORATION; WO2006/44762; (2006); A2;,
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Related Products of 2854-16-2, 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. 2854-16-2, name is 1-Amino-2-methylpropan-2-ol. A new synthetic method of this compound is introduced below.

To a solution of 2-bromobenzaldehyde (25 g, 135 mmol) in methanol (250 mL) was added l-amino-2-methylpropan-2-ol (12.04 g, 135 mmol) and NaOH (13.51 mL, 13.51 mmol). The reaction mixture was stirred under nitrogen atmosphere for 1 h. Then NaBH4 (4.09 g, 108 mmol) was added portion wise for 10 min. It was stirred at 25 °C for 40 h. The reaction mixture was concentrated under reduced pressure. The residue was dissolved in ethyl acetate (500 mL) and washed with brine solution (300 mL). The organic layer was dried over anhydrous Na2S04, filtered and concentrated to give the title compound (28 g, 108 mmol, 80 percent yield). NMR (DMSO-d6, 400MHz): delta = 7.55 (ddd, J=19.7, 7.7, 1.1Hz, 2H), 7.33-7.39 (m, 1H), 7.18 (td, J=7.6, 1.6 Hz, 1H), 4.19 (s, 1H), 3.78 (s, 2H), 2.40 (s, 2H), 1.99 (s, 1H), 1.03-1.13 ppm (m, 6H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2854-16-2, 1-Amino-2-methylpropan-2-ol, and friends who are interested can also refer to it.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; ASTEX THERAPEUTICS LIMITED; BUDZIK, Brian W; LI, Peng; PERO, Joseph E.; GRIFFITHS-JONES, Charlotte Mary; HEIGHTMAN, Thomas Daniel; NORTON, David; WILLEMS, Hendrika Maria Gerarda; WOOLFORD, Alison Jo-Anne; (176 pag.)WO2018/109642; (2018); 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. 480449-99-8, name is Benzyl 3-hydroxycyclobutanecarboxylate. A new synthetic method of this compound is introduced below., HPLC of Formula: C12H14O3

Intermediate 33: benzyl 3-((methylsulfonyl)oxy)cyclobutanecarboxylate To a solution of benzyl 3-hydroxycyclobutanecarboxylate (Intermediate 32; 0.90 g; 4.4 mmol), Et3N (1.20 mL; 8.6 mmol) in DCM (50 mL) was added MsCl (0.40 mL; 5.2 mmol) under nitrogen. The reaction mixture was stirred for 1 hour, quenched with water (20 mL), and extracted with DCM (50 mL*2). The combined organic layers were dried over anhydrous Na2SO4, filtered, and concentrated to afford 1.24 g (100%) of the title compound as a yellow oil, which was used directly without further purification. 1H NMR (300 MHz, DMSO-d6) delta [ppm]: 7.45-7.28 (m, 5H), 5.16-5.07 (m, 2H), 4.93 (t, J=7.4 Hz, 1H), 3.16 (s, 3H), 2.86 (dd, J=16.7, 8.5 Hz, 1H), 2.67 (dtd, J=10.2, 7.5, 2.8 Hz, 2H), 2.44-2.28 (m, 2H).

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, 480449-99-8, Benzyl 3-hydroxycyclobutanecarboxylate.

Reference:
Patent; Crosignani, Stefano; Cauwenberghs, Sandra; Deroose, Frederik; US2015/133422; (2015); A1;,
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Reference of 28539-02-8, 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.28539-02-8, name is 1-(Hydroxymethyl)benzotriazole, molecular formula is C7H7N3O, molecular weight is 149.15, as common compound, the synthetic route is as follows.

Preparation Example 144 To a mixture of 5-(piperidin-4-yl)-1,3-thiazol-2-amine hydrochloride (519 mg), dichloromethane (5 mL), and methanol (5 mL), 1H-benzotriazol-1-ylmethanol (423 mg), sodium acetate (388 mg), and sodium triacetoxy borohydride (1.0 g) in that order were added followed by stirring at room temperature for 2 hours. To the reaction mixture, a saturated aqueous sodium hydrogen carbonate solution and basic silica gel were added followed by concentration of the solvent under reduced pressure. The resulting residue was purified by basic silica gel column chromatography (chloroform/methanol) to give 5-(1-methylpiperidin-4-yl)-1,3-thiazol-2-amine (411 mg).

The chemical industry reduces the impact on the environment during synthesis 28539-02-8, I believe this compound will play a more active role in future production and life.

Reference:
Patent; KOTOBUKI PHARMACEUTICAL CO., LTD.; Astellas Pharma Inc.; Kameda, Minoru; Kuriwaki, Ikumi; Iikubo, Kazuhiko; Hisamichi, Hiroyuki; Kawamoto, Yuichiro; Moritomo, Hiroyuki; Suzuki, Tomoyuki; Futami, Takashi; Suzuki, Atsushi; Tsunoyama, Kazuhisa; Asaumi, Makoto; Tomiyama, Hiroshi; Noda, Atsushi; Iwai, Yoshinori; Tokuzaki, Kazuo; Okada, Haruki; Miyasaka, Kozo; US2014/142084; (2014); A1;,
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Synthetic Route of 63478-76-2, 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. 63478-76-2, name is 6-Heptyn-1-ol, molecular formula is C7H12O, 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 6-heptynol (331 mg, 2.95 mmol) in 10 ml of methanol was added KOH in 5 ml of H2O. After 10 min, iodine (824 mg, 3.24 mmol) was added at 0 C. and warmed to rt and stirred for 2 hr. The reaction was then quenched with water and extracted with ether (20 ml three times). The solvent was removed in vacuo, the residue dissolved in CH2Cl2, washed with brine and dried over MgSO4. Purification by silica gel chromatography (hexane:ethyl acetate=4:1) gave the product 498 mg (71% 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 63478-76-2, 6-Heptyn-1-ol.

Reference:
Patent; Iowa State University Research Foundation, Inc.; US2005/272954; (2005); A1;,
Alcohol – Wikipedia,
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Application of 4704-94-3, 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 4704-94-3, name is 2-(Hydroxymethyl)propane-1,3-diol. This compound has unique chemical properties. The synthetic route is as follows.

Production Example 10-15-Hydroxymethyl-1,3-dioxane To a dichloromethane (4.9 mL) suspension of 2-hydroxymethyl-1,3-propanediol (1.00 g, 9.41 mmol), were added formaldehyde dimethyl acetal (2.94 mL, 33.3 mmol), lithium bromide (159 mg, 1.84 mmol) and p-toluenesulfonic acid monohydrate (160 mg, 0.843 mmol), and the mixture was stirred at room temperature for three days. To the mixture, was added triethylamine (1.0 mL), the solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography to obtain the title compound (380 mg, 3.22 mmol) from fraction of n-heptane:ethyl acetate (4:1).1H-NMR (400 MHz, CDCl3) delta: 1.55 (br.s, 1H), 1.92-2.00 (m, 1H), 3.75 (dd, J=4.8, 6.8 Hz, 2H), 3.79 (dd, J=6.0, 11.6 Hz, 2H), 4.01 (dd, J=4.0, 11.6 Hz, 2H), 4.80 (d, J=6.4 Hz, 1H), 4.86 (d, J=6.4 Hz, 1H).

According to the analysis of related databases, 4704-94-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Eisai R&D Management Co., Ltd.; US2011/86882; (2011); A1;,
Alcohol – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 23377-40-4, 3-(Hexadecyloxy)propan-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: 23377-40-4, blongs to alcohols-buliding-blocks compound. SDS of cas: 23377-40-4

Oxalylchloride (2.04 mL, 3 eq., 23.8 mmol) was added to a solution of dimethyl allylphosphonate (1 .19 g, 1 eq., 7.9 mmol) in dichloromethane (35 mL). This mixture was gently refluxed during 3 days at 45C. After evaporation of all volatiles, the crude compound was diluted in 35 mL of dichloromethane. Hexadecyloxypropyl alcohol (2.5 g, 1 .05 eq., 8.3mmol) and freshly distilled triethylamine (1 .6 mL, 1 .5 eq., 20 mmol) were then added subsequently and the resulting solution was refluxed during 3 days at 45C. The volatiles were removed under reduced pressure, and the residue was purified by flash column chromatography (eluting PE/EtOAc 9:1 – 6:4 – 0:1 ) to afford 209 as a white amorphous solid. (2.52 g, 76%) 1H NMR (400 MHz, CDCI3) d 5.75 (m, 1 H, CH=CH2), 5.23 (m, 2H, CH2-CH=CH2), 4.13 (dt, J = 6.5, 1 .7 Hz, 2H, He), 3.73 (d, J = 10.9 Hz, 3H, 0-CH3), 3.48 (t, J = 6.2 Hz, 2H, Ha), 3.38 (t, J = 6.7 Hz, 2H, CH2-0), 2.62 (ddt, J = 22.0, 7.4, 1 .1 Hz, 2H, CH2-P), 1 .91 (p, J = 6.3Hz, 2H, CH2-b), 1 .54 (p, J = 6.9 Hz, 2H, CH2-CH2-0), 1 .32-1 .22 (m, 26H, CH2), 0.87 (t, J= 6.8 Hz, 3H, CH3). 31P NMR (162 MHz, CDC ) d 28.3. CAS: 1258789-65- 9

At the same time, in my other blogs, there are other synthetic methods of this type of compound,23377-40-4, 3-(Hexadecyloxy)propan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; CENTRE NATIONAL DE LA RECHERCHE SCIENTIFIQUE; UNIVERSITE D’ORLEANS; NEOVIRTECH; AGROFOGLIO, Luigi; ROY, Vincent; DE SCHUTTER, Coralie; BESSIERES, Maxime; GALLARDO, Franck; (93 pag.)WO2019/206907; (2019); 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.33420-52-9, name is 2,2-Difluoropropan-1-ol, molecular formula is C3H6F2O, molecular weight is 96.076, as common compound, the synthetic route is as follows.Recommanded Product: 33420-52-9

Step 4 (ME-54):A solution of crude ME-53 (3.8 g, 39.58 mmol) in Dimethyl formamide (5 mL) was added to asuspension of sodium hydride (60%; 1 .3 g, 32.5 mmol) in dry dimethyl formamide (20 mL) at 0C and the mixture was stirred at room temperature for 1 h. The reaction mass was again cooled to 0C and a solution of 5-bromo-2-fluoro benzonitrile (2.36 g, 11.8 mmol) in dimethyl formamide (5 mL) was added. The reaction mass was warmed to room temperature and stirred for 30 mm, quenched with saturated ammonium chloride solution and extracted withdiethyl ether. The combined organic layer was washed successively with water, brine; dried over anhydrous sodium sulfate and concentrated in vacuum to afford the crude intermediate. Purification by column chromatography over silica gel (60-l20mesh) and using 8% ethyl acetate in pet ether as the eluent afforded 2.5 g (69.4%) of ME-S4 as a yellow gummy liquid.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,33420-52-9, 2,2-Difluoropropan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; PROBIODRUG AG; HEISER, Ulrich; BUCHHOLZ, Mirko; SOMMER, Robert; DEMUTH, Hans-Ulrich; WO2014/140279; (2014); A1;,
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Application of 2919-23-5, 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. 2919-23-5, name is Cyclobutanol, molecular formula is C4H8O, 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.

a. 2-Cyclobutoxy-5-nitro-pyridine A mixture of 2-chloro-5-nitropyridine (7.12 g, 45.0 mmol) and cyclobutanol (3.40 g, 47.2 mmol) in THF (30 mL) was vigorously stirred at 0 C. while NaH (1.18 g, 46.7 mmol) was added in three portions over ~10-20 s under air (Caution: Extensive gas evolution). Reaction residue was rinsed down with additional THF (5 mL), followed by stirring under positive argon pressure in the ice bath for 1-2 more minutes. The ice bath was then removed and the brown homogeneous solution was stirred for 1 h. The reaction mixture was concentrated under reduced pressure at 80 C., taken up in 0.75 M EDTA (tetrasodium salt) (150 mL), and extracted with CH2Cl2 (1*100 mL, 1*50 mL). The combined organic layers were dried (Na2SO4), concentrated, taken up in MeOH (2*100 mL) and concentrated under reduced pressure at 60 C. to provide the title compound as a thick dark amber oil that crystallized upon standing (7.01 g, 80%). 1H NMR (CDCl3) delta 9.04 (dd, J=2.84 and 0.40 Hz, 1H), 8.33 (dd, J=9.11 and 2.85 Hz, 1H), 6.77 (dd, J=9.11 and 0.50 Hz, 1H), 5.28 (m, 1H), 2.48 (m, 2H), 2.17 (m, 2H), 1.87 (m, 1H), 1.72 (m, 1H).

According to the analysis of related databases, 2919-23-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Gaul, Michael David; Xu, Guozhang; Baumann, Christian Andrew; US2006/281764; (2006); A1;,
Alcohol – Wikipedia,
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Reference of 15484-46-5 ,Some common heterocyclic compound, 15484-46-5, molecular formula is C5H8O3, 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 la (3.48 g, 30 mmol) was dissolved in 50 mL of dry THF with imidazole (2.250 g, 33 mmol). TBDPSCI (9.070 g, 33 mmol) was added to the solution dropwise at 0 C. The reaction was stirred overnight at room temperature. Then, precipitate was removed by filtration to achieve clear solution which was further extracted with saturated sodium bicarbonate solution, water and brine. The organic layers were combined and dried over anhydrous sodium sulfate. (0396) The solution was collected, concentrated and subjected to flash chromatography to afford compound 8a. Yield, 6.99 g, 66%. -NMR (400 MHz, CDCl3): 5(ppm) 7.64-7.69 (m, 4H), 7.34-7.47 (m, 6H), 6.33(q, J= 1.9 Hz, 1H), 6.1 l(q, J=l.9 Hz, 1H), 4.42 (t, J=2. l Hz, 2H), 3.70 (s, 3H), 1.08 (s, 9H). 13C-NMR (100 MHz, CDCb): 5(ppm) 166.25, 139.33, 135.46, 133.24, 129.78, 127.77, 124.09, 62.21, 51.63, 26.82, 19.30. MS (m/z): [M]+ calcd. for C2, H2(,(LSI. 354.17; found, 377.1 for [M+Na]+.

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. 15484-46-5, Methyl 2-(hydroxymethyl)acrylate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; UNIVERSITY OF MASSACHUSETTS; THAYUMANAVAN, Sankaran; VACHET, Richard, W.; ZHUANG, Jiaming; ZHAO, Bo; (0 pag.)WO2020/6340; (2020); A1;,
Alcohol – Wikipedia,
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