Month: July 2021

Adding a certain compound to certain chemical reactions, such as: 349-95-1, (4-(Trifluoromethyl)phenyl)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, Recommanded Product: (4-(Trifluoromethyl)phenyl)methanol, blongs to alcohols-buliding-blocks compound. Recommanded Product: (4-(Trifluoromethyl)phenyl)methanol

General procedure: Aq ammonia (28%, 0.5 mmol), the appropriate alcohol 10 (3.4mmol), the catalyst 3 (1 mol% Ir), and the phthalate pH standard solution(0.5 mL, pH 4.01) were mixed in a microwave vial tube at 23 C under air. The vial was sealed with a cap, and the reactionmixture was stirred at 150 C for 24 h in a microwave reactor (25-32 W). After cooling to 23 C, aq NaOH (0.1 M, 1 mL) was addedto the mixture and extracted with EtOAc (3 × 2 mL). The combinedorganic layers were concentrated. The crude product was purifiedby column chromatography over silica gel eluting with hexane-EtOAc (98:2 to 9:1) or CHCl3 to afford the corresponding N-alkylatedamine 11l,o-s

At the same time, in my other blogs, there are other synthetic methods of this type of compound,349-95-1, (4-(Trifluoromethyl)phenyl)methanol, and friends who are interested can also refer to it.

Reference:
Article; Yamada, Yoichim. A.; Ohta, Hidetoshi; Yuyama, Yoshinari; Uozumi, Yasuhiro; Synthesis; vol. 45; 15; (2013); p. 2093 – 2100;,
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Reference of 6966-10-5, 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. 6966-10-5, name is (3,4-Dimethylphenyl)methanol. A new synthetic method of this compound is introduced below.

Example 39; 3′,4′-Dimethvlphenylmethyl 2-cvanopvrazolidine-1 -carboxylate (39)3′,4′-Dimethylphenylmethyl chloroformate was prepared by dissolving 3,4-dimethylbenzyl alcohol (94.0 mg, 0.69 mmol) was in 3 ml_ dichloromethane followed by diisopropylethylamine (145 uL, 0.83 mmol). 20% Phosgene in toluene (473 uL, 0.83 mmol) was added dropwise and the reaction mixture was allowed to stir at room temperature for 2 hours.4 was prepared according to Example 4. To this was added the 4′-acetylaminophenyl chloroformate in one portion and the reaction mixture was stirred overnight at room temperature. After removal of solvent by rotary evaporation, the title compound was purified by silica gel chromatography (CombiFlash, 20% ethyl acetate in hexanes to 100% ethyl acetate over 10 minutes.) The appropriate fractions were collected, combined and evaporated to dryness to yield 39 (57.0 mg, 31.9%), ESMS 260.4 (M+H+).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,6966-10-5, (3,4-Dimethylphenyl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; GLAXO GROUP LIMITED; WO2006/94003; (2006); A1;,
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Electric Literature of 19936-14-2, 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 19936-14-2 as follows.

To a solution of 5.66 g of 1-(4-bromophenyl)-cyclobutanol (24.92 mmol, described in example S2-A) in 70 ml DCM were added 4.23 g of (diethylamino)sulfur trifluoride (95%, 24.92 mmol) at 0 C. The reaction mixture was stirred at 0 C. for 35 min, then sat. NaHCO3- solution was added and the resulting mixture was extracted with DCM. The combined organic extracts were washed with brine, dried (MgSO4), filtered, and concentrated in vacuo to give a residue which was purified by flash column chromatography (100% pentane) to give 1-bromo-4-(1-fluoro-cyclobutyl)-benzene (3.66 g, 64%) as a colorless liquid.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,19936-14-2, its application will become more common.

Reference:
Patent; Conte, Aurelia; Kuehne, Holger; Luebbers, Thomas; Mattei, Patrizio; Maugeais, Cyrille; Mueller, Werner; Pflieger, Philippe; US2007/185058; (2007); A1;,
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Electric Literature of 722-92-9, Adding some certain compound to certain chemical reactions, such as: 722-92-9, name is 2-(4-Aminophenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol,molecular formula is C9H7F6NO, 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 722-92-9.

11091] To a solution of 2-(4-aminophenyl)-1,1,1,3,3,3- hexafluoropropan-2-ol (2.50 g, 9.64 mmol) (preparation, for example, W. A. Sheppard, J Am. Chem. Soc. 1965, 87, 24 10-2420) in glacial acetic acid (40 ml) was added, at RT, N-chlorosuccinimide (2.71 g, 20.2 mmol). The mixture was stirred at 75° C. for 3 h and then at RT for 14 h. Subsequently, the mixture was added to water and extracted with EtOAc. The organic phase was washed with water and saturated aqueous NaHCO3 solution and dried over magnesium sulphate. Afier solvent had been removed, the residue was taken up in MTI3E and the solids were filtered off. The filtrate was concentrated under reduced pressure and the crude product was purified by means of column chromatography on 5i02 (n-hexane/EtOAc gradient). 2.89 g (91percent) of 2-(4-amino-3,5-dichlorphenyl)- 1,1,1 ,3,3,3-hexafluoropro- pan-2-ol were obtained.11092] HPLCMSa): log P=3.04, mass (m/z)=328 [M+H].11093] ?H NMR (400 MHz, d3-acetonitrile): oe=5.13 (br s, 2H), 6.02 (br s, 1H), 7.51 (s, 2H).

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:
Patent; BAYER CROPSCIENCE AKTIENGESELLSCHAFT; HALLENBACH, WERNER; SCHWARZ, HANS-GEORG; ILG, KERSTIN; GOERGENS, ULRICH; KOEBBERLING, JOHANNES; TURGERG, ANDREAS; BOEHNKE, NIELS; MAUE, MICHAEL; VELTEN, ROBERT; HARSCHNECK, TOBIAS; HAHN, JULIA JOHANNA; HORSTMANN, SEBASTIAN; (160 pag.)US2016/278379; (2016); A1;,
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Adding a certain compound to certain chemical reactions, such as: 3279-95-6, 2-(Aminooxy)ethanol, 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: 3279-95-6, blongs to alcohols-buliding-blocks compound. Recommanded Product: 3279-95-6

The oxime compound, (E)-3,4-difluoro-2-(2-fluoro-4-iodo-phenylamino)-N-(2-hydroxy-ethoxy)-5-[(2-hydroxy-ethoxyi mino)-methyl]-benzamide obtained in Step B of Example 6 may be easily prepared from 3,4-difluoro-2-(2-fluoro-4-iodo-phenylamino)-5-formyl-N-(2-hydroxy-ethoxy)-benzamide obtained in Step F of Example 1 by a reaction with 2-aminooxyethanol in THF at room temperature. Namely, 3,4-difluoro-2-(2-fluoro-4-iodo-phenylamino)-5-formyl-N-(2-hydroxy-ethoxy)-benzamide (1.37 g) and aminooxy ethanol (262 mg) were mixed in THF at room temperature for 12 hours, and then the solvent was evaporated to give 3,4-difluoro-2-(2-fluoro-4-iodo-phenylamino)-N-(2-hydroxy-ethoxy)-5-[(2-hydroxy-ethoxyimino)-methyl]-benzamide.

The synthetic route of 3279-95-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CHUGAI SEIYAKU KABUSHIKI KAISHA; EP1780197; (2007); A1;,
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Reference of 5339-85-5, 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. 5339-85-5, name is 2-(2-Aminophenyl)ethanol, molecular formula is C8H11NO, 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.

From the reaction solution, 0.24 g of the catalyst was recovered. The recovered catalyst was regenerated by supporting 12 mg (5wt%) of K2 CO3. The procedures of Example 1 was repeated except that the so regenerated catalyst was used. The conversion of 2-(o-aminophenyl)ethanol was 100% and the yield of indole was 87.7%.

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 5339-85-5, 2-(2-Aminophenyl)ethanol.

Reference:
Patent; Research Association for Utilization of Light Oil; US4757152; (1988); A;,
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Related Products of 456-47-3, 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. 456-47-3, name is 3-Fluorobenzyl alcohol. A new synthetic method of this compound is introduced below.

General procedure: Sodium hydride (60% in mineral oil, 0.04g, 1mmol) was added to a stirred solution of benzyl alcohol derivative (1mmol) in anhydrous N,N-dimethylformamide (3mL of DMF) at room temperature and stirring was continued for 1h. 2-Amino-3-chloropyrazine (10b, 0.13g, 1mmol) was added to the reaction mixture and the reaction mixture was stirred at 100C for 15h. After cooling, the solvent was evaporated and the residue was partitioned between water and dichloromethane. The organic layer was dried over sodium sulfate anhydrous, filtered, and concentrated. The residue was purified by column chromatography (SiO2, EA/n-Hex=1/5). 4.1.2.1 3-(3-Fluorobenzyloxy)pyrazin-2-amine (11e) (0027) Light orange solid, yield: 75.6%, 1H NMR (400MHz, DMSO-d6) delta=5.39 (2H, s, OCH2Ph), 6.36 (2H, br, NH2), 7.14 (1H, td, J=2.6Hz, 9.0Hz, ArH), 7.25 (1H, d, J=3.1Hz, ArH), 7.32 (1H, d, J=7.6Hz, ArH), 7.37-7.44 (2H, m, ArH), 7.49 (1H, d, J=3.1Hz, ArH).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,456-47-3, its application will become more common.

Reference:
Article; Park, Jung-eun; Elkamhawy, Ahmed; Hassan, Ahmed H.E.; Pae, Ae Nim; Lee, Jiyoun; Paik, Sora; Park, Beoung-Geon; Roh, Eun Joo; European Journal of Medicinal Chemistry; vol. 141; (2017); p. 322 – 334;,
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Related Products of 50595-15-8, 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. 50595-15-8, name is tert-Butyl 2-hydroxyacetate. A new synthetic method of this compound is introduced below.

A suspension of 6-bromo-N-(4-fluoro-phenyl)-nicotinamide (0.112 g, 0.38 mmol), tert-butyl glycolate (0.1 g, 0.76 mmol), and potassium tert-butoxide (0.85 g, 0.76 mmol) in THF (10 mL) was heated in a sealed tube at 70° C. After 6 h the reaction mixture was diluted with ethyl acetate and washed with water bicarbonate and dried over sodium sulfate. Removal of the solvents provided a solid. Purification by reverse phase chromatography gave 0.010 g (8percent) of the titled product as a white solid; MS (EI) m/z 345.21 (M-H)-.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,50595-15-8, tert-Butyl 2-hydroxyacetate, and friends who are interested can also refer to it.

Reference:
Patent; Darwin Molecular Corporation; US6777432; (2004); B1;,
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Related Products of 3279-95-6, Adding some certain compound to certain chemical reactions, such as: 3279-95-6, name is 2-(Aminooxy)ethanol,molecular formula is C2H7NO2, 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 3279-95-6.

General procedure: 4a-c (1 equiv) were dissolved in ethanol (10mL). O-(2-hydroxyethyl)hydroxylamine (14, 2 equiv), acetic acid (2 equiv), pyridine (2 equiv) were added to the solution. After being refluxed for 5h, ethanol was removed under reduced pressure. The products were extracted with CH2Cl2. The combined extracts were washed with 2M HCl aqueous solution and brine. The organic layer was dried with anhydrous Na2SO4. The solvent was removed under reduced pressure and the residue was purified by column chromatography (PE: EtOAc=6: 1) to yield 15a-c. 3alpha-O-(2,3,4,6-tetra-O-benzoyl-beta-d-glucopyranosyl)-17-(O-(2-hydroxyethyl)oxime)-5beta-androstane (15a). The title compound was obtained starting from 4a (600mg, 0.69mmol) (white solid, 530mg, 82.8% yield, mp 91-94C). Analytical data for 15a: ESI-MS m/z (%) 950.4 [M+Na]+; 1H NMR (400MHz, CDCl3) delta 7.87-7.67(m, 8H, Bz-H), 7.48-7.18(m, 12H, Bz-H), 5.76 (t, J=9.7Hz, 1H, H-3?), 5.49 (t, J=9.7Hz, 1H, H-2?), 5.39-5.28 (m, 1H, H-4?), 4.80 (d, J=7.9Hz, 1H, H-1?), 4.41 (m, 2H, H-6?), 3.95 (m, 3H, H-5?, =NOCH2CH2OH), 3.72 (m, 2H, =NOCH2CH2OH), 3.49 (m, 1H, H-3), 2.28 (m, 2H, H-16), 1.73-0.85 (m, 20H), 0.73 (s, 3H, 18-CH3), 0.70 (s, 3H, 19-CH3).

According to the analysis of related databases, 3279-95-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Li, Haihong; Wang, Ke; Wan, Qi; Chen, Ying; Steroids; vol. 141; (2019); p. 81 – 95;,
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Adding a certain compound to certain chemical reactions, such as: 3562-73-0, 1-(4-Biphenylyl)ethanol, 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: 1-(4-Biphenylyl)ethanol, blongs to alcohols-buliding-blocks compound. name: 1-(4-Biphenylyl)ethanol

h): Take a reaction tube and add sodium azide 49mg.1-[4-(1,1′-biphenyl)]ethanol 59.5 mg,400 uL of trifluoroacetic acid, 150 uL of methanesulfonic acid, 1.0 mL of n-hexane, and stirred at 50 C for 36 hours.After the reaction was completed, 10 mL of a sodium hydroxide solution was added to quench the reaction, and the mixture was extracted with ethyl acetate three times.The organic phase was washed with 5 mL of brine, and the organic phases were combined and separated by column chromatography to obtain 45.7 mg of p-phenylaniline.The yield was 90%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,3562-73-0, 1-(4-Biphenylyl)ethanol, and friends who are interested can also refer to it.

Reference:
Patent; Peking University; Jiao Ning; Liu Jianzhong; (27 pag.)CN109134267; (2019); A;,
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