Month: August 2021

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 2043-47-2, name is 1H,1H,2H,2H-Nonafluoro-1-hexanol. This compound has unique chemical properties. The synthetic route is as follows. Recommanded Product: 1H,1H,2H,2H-Nonafluoro-1-hexanol

To a solution of the perfluoroalkyl alcohol (10 mmol) in 10 mLof dry THF, was added sodium hydride (60% 1.4 equiv. dissolved in 2 mL of dry THF in oil) at 0 C under nitrogen atmosphere. The mixture was stirred for 30 min. Then 1.35 g (10 mmol) of henylisothiocyanate was added. The reaction mixture was allowed to warm to room temperature and stirred for 3 h. The mixture was quenched with saturated aqueous ammonium chloride. The aqueous layer was washed with diethyl ether and the combined organic layers were dried over Na2SO4. The solvent was removed by vacuum evaporation and the crude products were purified with column chromatography on silica gel (70-230 meshes) using petroleum ether/diethyl ether (8:2) as eluent or recrystallized in cyclohexane to give the corresponding O-perfluoroalkyl thiocarbamate.

With the rapid development of chemical substances, we look forward to future research findings about 2043-47-2.

Reference:
Article; Chniti, Ines; Sanhoury; Chehidi; Journal of Fluorine Chemistry; vol. 156; (2013); p. 101 – 105;,
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Application of 34598-50-0, 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.34598-50-0, name is 5-Bromo-2,3-dihydro-1H-inden-1-ol, molecular formula is C9H9BrO, molecular weight is 213.07, as common compound, the synthetic route is as follows.

Commercially available 5-bromoindanone (5.1 g, 24.3 mmol) was diluted into methanol (150 mL), cooled to 0 0C, and treated with sodium borohyd?de (1.8 g, 48.6 mmol). The reaction mixture was warmed to room temperature, aged overnight, and then partitioned between water and methylene chloride, the organic phase separated, dried and concentrated in vacuo. The clean crude alcohol (5.0 g, 97%) was isolated and used in the next step without purification. This hydroxybromoindane (5.04 g, 23.6 mmol) was diluted into toluene (100 mL), treated with catalytic p-toluenesulfomc acid (400 mg), and the reaction mixture refluxed under Dean-Stark trap conditions for 6 h. The mixture was cooled to room temperature, extracted with saturated aqueous sodium bicarbonate, and the organic phase separated, d?ed and concentrated in vacuo. The clean crude bromoindene (4.6 g, 100%) was isolated as an oil and used in the next step without purification. This bromoindene (4.5 g) was diluted into (1 : 1) methanol-methylene chloride (150 mL), chilled to -78 0C, and treated with ozone for 30 minutes, removed from the ozonator, warmed to room temperature, and treated with solid sodium bicarbonate (2.5 g) and dimethylsulfide (3 mL). The reaction mixture was aged for 14 h, treated with 78% ammonium hydroxide in water (30 mL), and the mixture maintained at room temperature overnight. The reaction mixture was then concentrated in vacuo, re-dissolved in ethyl acetate, washed with saturated aqueous sodium bicarbonate, and the organic phase separated, dried and concentrated in vacuo. The crude product was purified by flash column chromatography (Biotage, SiO2, 20% EtOAc-heptane) to provide the solid bromoisoqumolme. EXAMPLE 59 was prepared from this bromoisoqumohne by first Heck coupling in a similar manner as described in EXAMPLE 53 above and illustrated in Scheme 8. The resultant lsoquinohne acrylamide methyl ester intermediate was saponified with LiOH, and the acid reduced with p-toluenesulfonyl hydrazide, both in a similar manner as described in the examples above to provide the desired product. LCMS m/z 321 (M++ 1)

Statistics shows that 34598-50-0 is playing an increasingly important role. we look forward to future research findings about 5-Bromo-2,3-dihydro-1H-inden-1-ol.

Reference:
Patent; MERCK & CO., INC.; WO2006/52555; (2006); A2;,
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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.2568-33-4, name is 3-Methylbutane-1,3-diol, molecular formula is C5H12O2, molecular weight is 104.1476, as common compound, the synthetic route is as follows.Computed Properties of C5H12O2

To 3-methylbutane-1,3-diol (0.1 g, 0.98 mmol) was added potassium t-butoxide (0.94 mL, 1M in THF) and stirred for 10 minutes. Example 1E (0.2 g, 0.47 mmol) in 1.2 mL of THF was added and the mixture stirred at ambient temperature for 30 minutes. The mixture was diluted with dichloromethane, 20 muL of glacial acetic acid was added and the resulting mixture was filtered, loaded onto silica and chromatographed. (0-20% MeOH in dichloromethane (0.1% NH4OH) over 900 mL) to afford the title compound (70 mg, 0.14 mmol, 29% yield). 1H NMR (300 MHz, CDCl3) delta ppm 1.30 (s, 6H), 1.41 (s, 9H), 1.67-1.92 (m, 3H), 1.94-2.09 (m, 3H), 3.60-3.81 (m, 2H), 3.85 (s, 3H), 4.11-4.23 (m, 1H), 4.23-4.33 (m, 3H), 4.54 (dd, J=15.1, 2.9 Hz, 1H), 6.98 (d, J=8.5 Hz, 1H), 7.01 (s, 1H), 7.53 (dd, J=8.6, 2.2 Hz, 1H), 8.26 (d, J=2.4 Hz, 1H). MS (DCI/NH3) m/z 512.3 (M+H)+. Analytical calculated for C26H36F3N3O4.0.2H2O: C, 60.56; H, 7.13; N, 8.15. Found: C, 60.57; H, 7.25; N, 8.12

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2568-33-4, 3-Methylbutane-1,3-diol, and friends who are interested can also refer to it.

Reference:
Patent; ABBOTT LABORATORIES; US2010/69348; (2010); A1;,
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Synthetic Route of 162744-59-4, 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. 162744-59-4, name is (4-Bromo-2,6-difluorophenyl)methanol, molecular formula is C7H5BrF2O, 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.

Step 1: The preparation of 2,6-difluoro-4-bromobenzyl methanesulphonate; 2,6-difluoro-4-bromobenzyl alcohol (9.50 g) and triethylamine (5.0 g) were dissolved in THF cooled to 10C with stirring. Methanesulphonyl chloride (4.8 g) was added in a solution of THF (10ml) over 10 minutes, and a white solid precipitated from the solution. The reaction was then warmed to room temperature for one hour and then the solid was collected and washed with diethyl ether. The filtrate was evaporated to give 2,6-difluoro-4- bromobenzyl methanesulphonate (13.0 g) as a golden oil which slowly crystallised. ¹H NMR (CDCl3) No. ppm: 3.05 (s, 3H), 5.3 (s, 2H), 7.15 (t,2H).

According to the analysis of related databases, 162744-59-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SYNGENTA PARTICIPATIONS AG; SYNGENTA LIMITED; WO2005/123698; (2005); A1;,
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Electric Literature of 1450754-41-2, Adding some certain compound to certain chemical reactions, such as: 1450754-41-2, name is 2-(3-But-3-ynyl-3H-diazirin-3-yl)-ethanol,molecular formula is C7H10N2O, 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 1450754-41-2.

(f) Imidazole (740 mg, 10.87 mmol, 3.0 eq), triphenylphosphine (1.05 g, 3.99 mmol, 1.1 eq) and dichloromethane (5 ml) were added to the reaction flask and cooled to 0 C.Add iodine (1.1 g, 4.35 mmol, 1.2 eq), and add the incubation reaction for 30 minutes.A solution of compound 5 (500 mg, 3.62 mmol, 1 eq) in dichloromethane (1 ml) was added at low temperature, and the mixture was stirred for 4 hours.Quenched with saturated sodium sulfite solution, extracted with ethyl acetate, dried and dried.Purified by column to obtain 400 mg of compound 6, yield: 46%

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. 1450754-41-2, 2-(3-But-3-ynyl-3H-diazirin-3-yl)-ethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Suzhouguangdian Biological Technology Co., Ltd.; Ni Runyan; Wang Wei; (8 pag.)CN109369532; (2019); A;,
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Adding a certain compound to certain chemical reactions, such as: 6214-44-4, (4-Ethoxyphenyl)methanol, 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: C9H12O2, blongs to alcohols-buliding-blocks compound. COA of Formula: C9H12O2

Reference Example 026 Preparation of Compound 46 (0606) (0607) Dibenzo-18-crown-6 (0.152 mg, 11.8 mmol) and potassium hydroxide (1.14 g, 20.3 mmol) were added to the toluene solution (30 mL) of Compound 38 (2.0 g, 8.44 mmol) and 4-ethoxybenzylalcohol (1.80 g, 11.8 mmol), and the mixture was stirred at 120 C. for 2 hours. Water was added to the mixture, and the mixture was extracted with chloroform. The organic layer was dried over magnesium sulfate. The solvent was condensed under reduced pressure. The residue was purified by silica gel chromatography (ethyl acetate-hexane) to afford Compound 46 (2.42 g, yield 93%). (0608) 1H-NMR (CDCl3) delta: 8.20 (d, J=2.4 Hz, 1H), 7.62 (dd, J=8.8, 2.5 Hz, 1H), 7.38-7.32 (m, 2H), 6.91-6.86 (m, 2H), 6.68 (d, J=8.7 Hz, 1H), 5.25 (s, 2H), 4.03 (q, J=7.0 Hz, 2H), 1.41 (t, J=7.0 Hz, 3H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,6214-44-4, (4-Ethoxyphenyl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; SHIONOGI & CO., LTD.; Matsumura, Akira; Kobayashi, Naotake; Nishiura, Yuji; Tagashira, Sachie; Kida, Shiro; Kurahashi, Kana; Yonehara, Mitsuhiro; US2015/246938; (2015); 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.38493-59-3, name is (3-Bromo-4-methoxyphenyl)methanol, molecular formula is C8H9BrO2, molecular weight is 217.06, as common compound, the synthetic route is as follows.name: (3-Bromo-4-methoxyphenyl)methanol

On the basis of Example 1, the other steps were not changed, and the method of step (2) in Example 1 was changed to 10 gCompound B,3-bromo-4-methoxybenzyl alcohol,Adding 8.6 g of m-chlorobenzeneboronic acid,18.8 g of potassium carbonate,Urea 82.8 mg,Palladium acetate 210 mg,Isopropyl alcohol / water solvent 100mL,Stir at room temperature. Until the solid completely dissolved, remove the reaction system of oxygen, anaerobic reaction, heating,After completion of the reaction, the isopropanol and part of the water were removed under reduced pressure, and then extracted with ethyl acetate. The organic layers were combined, dried over anhydrous sodium sulfate, and the palladium salt was removed by suction filtration. , 11.46 g, yield> 95%. The overall yield of this example was 65.5%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,38493-59-3, (3-Bromo-4-methoxyphenyl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; Xu Jiangping; Chen Yunfeng; Zhou Zhongzhen; (8 pag.)CN106632070; (2017); A;,
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Application of 17100-58-2, Adding some certain compound to certain chemical reactions, such as: 17100-58-2, name is (4-Bromo-2-methylphenyl)methanol,molecular formula is C8H9BrO, 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 17100-58-2.

Intermediate 168: [2′,3-dimethyl-4′-(trifluoromethyl)-4-biphenylyl]methanol; To a solution of (4-bromophenyl)-methanol (Intermediate 15, 2.0 g, 9.8 mmol) and the commercially available [2-methyl-4-(trifluoromethyl)phenyl]boronic acid (2 g, 9.8 mmol) in DME was added a 1 M solution of sodium carbonate (20 ml_, 2 equiv.) then Pd(PPh3)4 (120 mg, 0.01 equiv.) was added and the reaction mixture was heated at 800C for 18 hours. The reaction was filtered on Celite and washed with Et2O. The filtrate was then washed with water and a NaHCO3 solution, dried over sodium sulphate and concentrated in vacuo. The residue was purified by column chromatography on silica gel eluted with DCM and DCM/MeOH 95/5 to give the title compound. (2.3 g, yield: 84%). 1H NMR: (CDCI3) delta 7.60-7.4 (m, 3H), 7.35 (d, 1 H), 7.2-7.1 (m, 2H), 4.75 (s, 1 H), 2.45 (s, 3H), 2.35 (s, 3H).

According to the analysis of related databases, 17100-58-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; BOUILLOT, Anne Marie Jeanne; DODIC, Nerina; GELLIBERT, Francoise Jeanne; MIRGUET, Olivier; WO2010/15652; (2010); A2;,
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Related Products of 41175-50-2, 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. 41175-50-2, name is 1,2,3,5,6,7-Hexahydropyrido[3,2,1-ij]quinolin-8-ol, molecular formula is C12H15NO, 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.

Phosphorous oxychloride (2.7 mL, 4.4 g, 29 mmol) was added dropwise in flask containing 10 mL DMF for a period of 15 min at 4 C. A solution of 8-hydroxyjulolidine 7 (5.15 g,26.9 mmol) in DMF (5 mL) was then added dropwise to the complex over period of 10 min. When the addition was complete,the reaction was stirred at room temperature for 30 min,and then heated at 100 C for 30 min. After cooling to room temperature, 30 mL of water was added to the stirred dark solution. The aqueous mixture was stirred for 1.5 h resulting in the formation of a blue-green precipitate. The precipitate was isolated by filtration, washed with water and dried. The crude product was purified by column chromatography on silica gel(Toluene/EtOAc, 2:1) Yield = 94 %, m.p. 73-74 C

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 41175-50-2, 1,2,3,5,6,7-Hexahydropyrido[3,2,1-ij]quinolin-8-ol.

Reference:
Article; Chemate, Santosh B.; Sekar, Nagaiyan; Journal of Fluorescence; vol. 25; 6; (2015); p. 1615 – 1628;,
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Synthetic Route of 13330-96-6, 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 13330-96-6 as follows.

General procedure: To a solution of 6-substituted pyridazinone 9 (0.5 mmol) in DMF (10 mL) was added Cs2CO3 (0.55 mmol). An appropriately substituted nitro benzyl chloride (0.52 mmol) was added and the resulting mixture was stirred at 40-50 C for 3 h, the solvent was removed under reduced pressure and the residue was dissolved in EtOAc (30 mL), which was then washed with brine (3 × 10 mL). The organic layer was dried over anhydrous Na2SO4 and concentrated in vacuo. The crude product, 2-nitrobenzyl-6-substituted-pyridazin-3(2H)-one (10), was used in the next step without further purification. To a solution of 10 in 95 % ethanol (50 mL) was added acetic acid (10 mmol) followed by slow addition of iron powder (2 mmol). The resulting mixture was stirred for 5 h at 100 C. The mixture was then filtered through celite and the filter cake was washed with 95 % ethanol (3 × 15 mL). The combined ethanol filtrates were evaporated in vacuo and the residue was re-dissolved in ethyl acetate (30 mL). The organic layer was washed with brine (3 × 10 mL) and 2 M NaOH (10 mL) sequentially. The organic layer was dried over anhydrous Na2SO4, evaporated in vacuo to afford 2-aminobenzyl-6-substituted-pyridazin-3(2H)-one (11) as a yellow solid, which was used without further purification. To a stirred solution of 11 and triphosgene (1 mmol) in dry dichloromethane (5 mL) was added triethylamine (2 mmol) under nitrogen atmosphere. A solution of the corresponding alcohol (1 mmol) in dichloromethane (5 mL) was added 5-10 min later and the mixture was stirred at room temperature overnight, diluted with dichloromethane (15 mL) and washed with water (3 × 20 mL). The organic phases were separated, combined, dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by using column chromatography to afford the corresponding product.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,13330-96-6, its application will become more common.

Reference:
Article; Xing, Weiqiang; Ai, Jing; Jin, Shiyu; Shi, Zhangxing; Peng, Xia; Wang, Lang; Ji, Yinchun; Lu, Dong; Liu, Yang; Geng, Meiyu; Hu, Youhong; European Journal of Medicinal Chemistry; vol. 95; (2015); p. 302 – 312;,
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