Author: tianli

Adding a certain compound to certain chemical reactions, such as: 83647-43-2, (3-Bromo-2-methylphenyl)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, Application In Synthesis of (3-Bromo-2-methylphenyl)methanol, blongs to alcohols-buliding-blocks compound. Application In Synthesis of (3-Bromo-2-methylphenyl)methanol

Perbromomethane (14.35 g, 43.3 mmol) was added portionwise to a solution of (3-bromo-2-methylphenyl)methanol (7.25 g, 36.1 mmol) and triphenylphosphine (11.35 g, 43.27 mmol) in DCM (120 mL) (reaction exotherms to ?40 C.) and the reaction was stirred at room temperature for 2 hours. The residue was passed through a pad of silica, eluting with DCM. The filtrate was concentrated to dryness, then the crude product was purified by flash silica chromatography, elution gradient 0 to 25% EtOAc in heptane. Product fractions were concentrated to dryness to afford 1-bromo-3-(bromomethyl)-2-methylbenzene (8.52 g, 90%) as a colourless oil. 1H NMR (500 MHz, CDCl3, 27 C.) 2.48 (3H, s), 4.52 (2H, s), 6.99-7.05 (1H, m), 7.22-7.27 (1H, m), 7.52 (1H, dd).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,83647-43-2, (3-Bromo-2-methylphenyl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; AstraZeneca AB; YANG, Bin; VARNES, Jeffrey Gilbert; SCOTT, James Stewart; MOSS, Thomas Andrew; O’DONOVAN, Daniel Hillebrand; NISSINK, Johannes Wilhelmus Maria; HUGHES, Samantha Jayne; BARLAAM, Bernard Christophe; (83 pag.)US2017/305909; (2017); A1;,
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Related Products of 80866-82-6 ,Some common heterocyclic compound, 80866-82-6, molecular formula is C8H9BrO2, 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.

(5-Bromo-2-methoxyphenyl)methanol (1.89 g, 8.71 mmol) was dissolved in 25 mL of dichloromethane. Imidazole (0.711 g, 10.45 mmol) was added, followed by addition of tert-butyldimethylsilyl chloride (1.378 g, 9.14 mmol). After stirring at room temperature for 15 minutes, the reaction was complete by thin layer chromatography. CH3OH (1 mL) was added and the reaction mixture was stirred for 5 minutes and was washed with 1 M aqueous HCl (3*15 mL) and brine (15 mL), and was dried over sodium sulfate. After filtration, the filtrate was concentrated to provide the title compound, which was used without additional purification. 1H NMR (400 MHz, Chloroform-d) delta ppm 7.60 (dd, J=2.5, 1.2 Hz, 1H), 7.33 (dd, J=8.7, 2.6 Hz, 1H), 6.71 (d, J=8.6 Hz, 1H), 4.74 (d, J=1.0 Hz, 2H), 3.82 (d, J=1.1 Hz, 3H), 0.99 (s, 9H), 0.15 (s, 6H); MS(ESI+) m/z=329.8 (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. 80866-82-6, 5-Bromo-2-methoxybenzyl alcohol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; AbbVie S.a.r.l.; Galapagos NV; Altenbach, Robert J.; Bogdan, Andrew; Couty, Sylvain; De Lemos, Elsa; Desroy, Nicolas; Duthion, Beranger; Gfesser, Gregory A.; Greszler, Stephen N.; Housseman, Christopher Gaetan; Koenig, John R.; Kym, Philip R.; Liu, Bo; Scanio, Marc J.; Searle, Xenia; Wang, Xueqing; Yeung, Ming C.; Zhao, Gang; (263 pag.)US2018/99931; (2018); A1;,
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Synthetic Route of 115-20-8, 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. 115-20-8, name is Trichloroethanol. A new synthetic method of this compound is introduced below.

To a suspension of (2-benzyloxy-3,5-dimethyl) phenoxyacetic acid (270 mg, 0.94 mmol) and 1,3-dicyclohexylcarbodimide (292.0 mg, 1.41 mmol) in CH2Cl2 (10.0 mL) was added pyridine (76.0 mL) and 2,2,2-trichloroethanol (117.0 mL). The suspension was stirred at room temperature for 12 h. The precipitation was filtered through filter paper and the filtrate was concentrated. Flash column (EtOAc in hexanes 5% to 10%) afforded 12c (311.1 mg) in 78.9% yield as an oil. [00783] 1H NMR (CDCl3) ¶7.52-7.28 (m, 5H, C6H5), 6.67 (s, 1H, C6H2), 6.60 (s, 1H, C6H2), 5.04 (s, 2H, CH2C6H5), 4.85 (s, 2H, OCH2CO), 4.84 (s, 2H, OCH2CCl3), 2.26 (s, 3H, CH3C6H2), 2.19 (s, 3H, CH3C6H2); 13C NMR d 167.6, 150.3, 144.4, 137.8, 133.4, 132.5, 128.3, 128.3, 127.8, 125.1, 125.1, 113.1, 94.4. 74.6, 74.0, 65.8, 21.1, 16.1.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,115-20-8, Trichloroethanol, and friends who are interested can also refer to it.

Reference:
Patent; University of Arkansas; US6657052; (2003); B1;,
Alcohol – Wikipedia,
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Application of 722-92-9 ,Some common heterocyclic compound, 722-92-9, molecular formula is C9H7F6NO, 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.

Intermcdiate H; 6-Chloro-3-(2-ethoxy-3,4-dioxo-cyclobut- 1 -enylamtno)-2-hydroxy-N-(4-{2,2,2-trif luoro-1 – hydroxy-l-triftuoromepsilonthyl-ethyl)-phenylj-benzenesulfonamide; HIi Preparation of Intermediate Ht; 2-rert-Butyl-6-chloro-ben*zooxazole-7-sul-:onic acid [4-{2,2,2-trifluoro-l -hydroxy-1 -trifluoromethyl-ethy I )~rhohenyl]-amide; 2-tert-Buryl-6-chJoro-ben20oxazole-7-sulfonyl chloride (500 mg, 1.62 mmo.) {prepared according to the procedure described in US 2007/067088 page 17} , 2-(4-aminophenyl)- l,l,l,3,3,3-hexafluoropropan-2-ol (420 mg, 1.62 mmol) and triethylamine (0.226 ml, 1.62 mmol) were combined in THF (5 ml) to give a yellow solution. The reaction, mixture was stirred at room temperature for 2 h then heated at 50 0C for 48 h. The reaction mixture was partitioned between EtOAc (20 ml) and IM HCI (10 ml), live organic layer was washed with brine (10 ml), dried (MgSO-O, filtered and added to silica gel (4 g) then carefully evaporated in vacuo. The silica gel was dry-loaded onto an (Isolure.(TM). Flash Si II 25 g) column for purification by chromatography, eluting with iso-hexane/ErOAc (10/1). The product fractions were combined and evaporated to dryness in vacuo to yield the title product. IH NMR 6H (400MHz DMSO) 8.55 (s, IH), 7.94 (d, IH), 7.61 (d, IH), 7.49 (d, 2H) 7.19 Patent; NOVARTIS AG; BAETTIG, Urs; BRUCE, Ian; PRESS, Neil John; WATSON, Simon James; WO2010/63802; (2010); A1;,
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Related Products of 96-35-5, 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. 96-35-5, name is Methyl 2-hydroxyacetate, molecular formula is C3H6O3, 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: Intermediate D15-2-hydroxyacetohydrazide A mixture of methyl 2-hydroxyacetate (9g, 0.1mol, 1equiv) and hydrazine hydrate (9.6ml, 1.5equiv, 85%) in methanol (100ml) was refluxed for 8h before methanol and exceesive hydrazine hydrate were evaporated. Toluene was added and evaporated again to remove the residual water to give the title compound as a white solid which could be used in next step without further purification.

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 96-35-5, Methyl 2-hydroxyacetate.

Reference:
Patent; Shanghai Institute of Materia Medica, Chinese Academy of Sciences; SHEN, Jianhua; WANG, Yiping; WANG, Kai; EP2725024; (2014); 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. 552331-15-4, name is 1-(5-Bromo-2-fluorophenyl)ethanol. A new synthetic method of this compound is introduced below., Computed Properties of C8H8BrFO

Step A: 4-bromo-2-( 1 -bromoethyl)- 1 -fluorobenzene (30-2)To a stirred solution of 1-(5-bromo-2-fluorophenyl)ethanol 30-1 (1.2 g, 5.48 mmol) in DCM (15 ml) was added tribromophosphine (0.26 mL, 2.74 mmol). The reaction mixture was stirred at 0C for lh, and then diluted with DCM (50 mL). Then saturated NaHCO3 solution was addeddropwise to the mixture, and the layers were separated. The organic layer was washed with saturated NaHCO3 solution (3OmL), brine (30 mL), and then dried over Na2SO4, and concentrated to give the crude product 30-2, which was used in the next step without purification.

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, 552331-15-4, 1-(5-Bromo-2-fluorophenyl)ethanol.

Reference:
Patent; MERCK SHARP & DOHME CORP.; HAGMANN, William, K.; NARGUND, Ravi, P.; BLIZZARD, Timothy, A.; JOSIEN, Hubert; BIJU, Purakkattle; PLUMMER, Christopher, W.; DANG, Qun; LI, Bing; LIN, Linus, S.; CUI, Mingxiang; HU, Bin; HAO, Jinglai; CHEN, Zhengxia; WO2014/22528; (2014); A1;,
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Synthetic Route of 928-92-7 ,Some common heterocyclic compound, 928-92-7, molecular formula is C6H12O, 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.

To a stirred solution of oxalyl chloride (5.23 mL 60 mmol) in 50 mL dry CH2Cl2 at -78°C under Argon, dimethyl sulfoxide ( 8.51 mL, 120 mmol) in 5 mL dry CH2Cl2 was added slowly. The reaction mixture was allowed to stirr for next 15 min. 4-Hexen-1-ol (4.7 mL, 40 mmol) in 10 mLCH2Cl2 was added dropwise to the reaction mixture and stirring was continued for next 45 min at -78°C. Further, Et3N (33.38 mL, 240 mmol) was added dropwise at 0°C and the reaction mixture was allowed to stirr for next 1 h (Foul smell of dimethyl sulfide). This was further treated with benzyl(triphenylphosphoranylidene)acetate (19.7 g, 48 mmol) in 70 mL dry CH2Cl2 and wasallowed to stirr for next 12 h at room temperature. Then, the reaction mixture was quenched withwater and extracted with excess CH2Cl2 and brine. The organic phase was separated, dried over MgSO4 and evaporated under reduced pressure. The crude brownish oil was subjected to column chromatography. The product (8) was separated as light yellow oil (95:5, E:Z) at gradient(hexane/ethyl acetate, 95:5) (7.73 g, 84percent).

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. 928-92-7, 4-Hexen-1-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Holla, Harish; Labaied, Mehdi; Pham, Ngoc; Jenkins, Ian D.; Stuart, Kenneth; Quinn, Ronald J.; Bioorganic and Medicinal Chemistry Letters; vol. 21; 16; (2011); p. 4793 – 4797;,
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Application of 4720-29-0 , The common heterocyclic compound, 4720-29-0, name is 3-(Benzylamino)-1-propanol, molecular formula is C10H15NO, 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.

1,1-bis(methylthio)-2-nitroethylene 9 (1.00 g, 6.06 mmol) was added to asolution of N-benzylamino-3-propan-1-ol 8a (1.00 g, 6.06 mmol) and DMAP (0.74 g, 6.06mmol) in t-butanol (20 mL). The resulting solution was heated to reflux for 24 h under nitrogenatmosphere. The reaction was monitored by TLC (CH2Cl2/MeOH, 97/3). After cooling to roomtemperature, the solvent was removed in vacuo to afford an oily residue which was purified byflash chromatography on silica gel (CH2Cl2/MeOH, 98/2) to give nitroacetamide 11a (oil, 0.42 g,28%), a mixture of (Z)- and (E)-isomers in a ratio close to 1/1.

The synthetic route of 4720-29-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Fante, Bamba; Soro, Yaya; Siaka, Sorho; Marrot, Jerome; Coustard, Jean-Marie; Synlett; vol. 25; 7; (2014); p. 969 – 974;,
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Synthetic Route of 2516-33-8 ,Some common heterocyclic compound, 2516-33-8, molecular formula is C4H8O, 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.

To a stirring solution/suspension comprised of N-hydroxyphthalimide (Aldrich, 57.15 g, 339.8 mmol), cyclopropanemethanol (Aldrich, 25.10 g, 341.1 mmol), and triphenylphosphine (“DEAD,” Aldrich, 91.0 g, 344 mmol) in 1.00 L of tetrahydrofuran under a nitrogen atmosphere and cooled to 6 C. (internal mixture temperature) with an ice-water bath was added diethyl azodicarboxylate (Aldrich, 56 ml, 356 mmol) dropwise over 20 minutes via addition funnel. The reaction mixture temperature was kept below 20 C. during the addition. Following addition of the DEAD, the cold bath was removed and the reaction mixture was stirred for 15 hours. The mixture was concentrated to a paste under reduced pressure. Chloroform (ca. 300 ml) was added and the mixture swirled to loosen all solids. Vacuum filtration removed the insolubles. The filtrate was likewise filtered to remove white precipitate that formed and to give a clear filtrate. Concentration under reduced pressure afforded a clear oil. Flash filtration through silica gel (100% chloroform) gave filtrates containing unseparated product. These filtrates were combined and concentrated under reduced pressure to afford 127.4 g of a clear oil. The oil was dissolved in absolute ethanol (400 ml) and the solution was refrigerated for two hours. A white crystalline solid had precipitated and was subsequently collected by vacuum filtration. The product was dried in the vacuum oven (60 C.) to afford 42.66 g (58%) of the desired material; m.p. 71-77 C.; 1H-NMR (400 MHz; CDCl3 signal offset to delta 6.96) delta 7.54-7.43 (m, 4H), 3.74 (d, 2H, J=7.6 Hz), 1.02-0.95 (m, 1H), 0.34-0.30 (m, 1H), 0.04-0.00 (m, 1H).

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. 2516-33-8, Cyclopropylmethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Warner-Lambert Company; US7030119; (2006); B1;,
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Related Products of 616-29-5, Adding some certain compound to certain chemical reactions, such as: 616-29-5, name is 1,3-Diaminopropan-2-ol,molecular formula is C3H10N2O, 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 616-29-5.

VII. 1 (3-tert-Butoxycarbonylamino-2-hydroxy-propyl)-carbamic acid tert-butyl esterDi-tert-butyl dicarbonate (41 .5g) was dissolved in dichloromethane (40.0 ml), a solution of 1 ,3- diamino-propan-2-ol (8.0g) and triethylamine (1 .5 ml) indichloromethane/methanol (1 :5; 100 ml) was added and the reaction mixture was stirred at room temperature overnight. The solution was concentrated in vacuo and the residue was dissolved in dichlormethane. The organic layer was washed with water, separated, dried and concentrated in vacuo. The residue was purfied by chromatography (silica / dichloromethane: methanol 25:1 ).Yield: 17 gESI mass spectrum: m/z = 291 (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. 616-29-5, 1,3-Diaminopropan-2-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; HECKEL, Armin; HIMMELSBACH, Frank; KLEY, Joerg; LEHMANN-LINTZ, Thorsten; REDEMANN, Norbert; SAUER, Achim; THOMAS, Leo; WIEDENMAYER, Dieter; BLACK, Phillip; BLACKABY, Wesley; LINNEY, Ian; AUSTEN, Matthias; DANILEWICZ, John; SCHNEIDER, Martin; SCHREITER, Kay; WO2011/104340; (2011); A1;,
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