Month: June 2021

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. 17773-10-3, name is Choline Iodide. A new synthetic method of this compound is introduced below., Safety of Choline Iodide

Preparation of Tetraalkylammonium Hydroxides; The above TAA halides were converted to the equivalent hydroxide using the anion exchange resin, Dowex 550. The general procedure is described in detail for the exchange of choline iodide to choline hydroxide. The resin (30 g) was activated using NaOH before being thoroughly washed with distilled water. To this was added [(CH3)3N(CH2CH2OH)]I (1.99 W 8 mmol) in distilled water (50 ml). This was then agitated on a mixing plate for 24 hours. The resin was removed by filtration and further washed with distilled water (4×15 ml). The filtrate and washings were reduced on a rotary evaporator to a volume of 8 ml. The filtrate was shown to contain no halide using the silver nitrate test. An aliquot of the solution (1 ml) was diluted with water (9 ml) and titrated with HCl (0.1M) to establish the hydroxide content as 1.0M.Calculated yield=0.96 g (99%) (1M solution)

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, 17773-10-3, Choline Iodide.

Reference:
Patent; PILKINGTON GROUP LIMITED; US2012/263903; (2012); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Reference of 3562-73-0, 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. 3562-73-0, name is 1-(4-Biphenylyl)ethanol. A new synthetic method of this compound is introduced below.

General procedure: Under an N2 atmosphere, a mixture of secondary alcohol (0.5 mmol), primary alcohol (0.6 mmol), 1a (5 mol %), NaOH (0.1 mmol), 4 A molecular sieve (0.6 g), and toluene (1.5 mL) was added into a 25 mL Schlenk tube equipped with a stirring bar. The mixture was heated to 120 C under a slow and steady N2 flow for 24 h. After cooling to ambient temperature, 6 mL water was added and the aqueous solution extracted with ethyl acetate (3 x 5 mL). The combined extracts were dried over anhydrous Na2SO4, and concentrated under reduced pressure. The crude product purified on a short flash chromatography column.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,3562-73-0, its application will become more common.

Reference:
Article; Zhang, Shi-Qi; Guo, Bin; Xu, Ze; Li, Hong-Xi; Li, Hai-Yan; Lang, Jian-Ping; Tetrahedron; vol. 75; 47; (2019);,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

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 23147-58-2, name is Glycerol aldehyde dimer. This compound has unique chemical properties. The synthetic route is as follows. SDS of cas: 23147-58-2

Example B39; 2-((2R,3aR,12bS)-2-[(dimethylamino)methyl]-11-fluoro-3,3a,8,12b-tetrahydro- dibenzo[3,4:6,7]cyclohepta[1,2-b]pyrrol-l(2H)-yl)ethanol (final compound 39); Hydroxyacetaldehyde dimer (2,5-dihydroxy-l,4-dioxane) (240 mg, 2.0 mmol) was dissolved in MeOH (25 mL) and stirred at 40C for 30 minutes, then amine compound 37 (124 mg, 0.40 mmol) was added and stirring at 40 C continued for another 30 minutes. After cooling down to room temperature, AcOH (120 mg, 2.0 mmol) was EPO added, followed by sodium cyanoborohydride (188 mg, 3.0 mmol) and the resulting mixture was stirred for 2 hours. After this time it was quenched with concentrated HCl (2 mL), treated with solid NaHCO3 (2.94 g, 35 mmol), IN sodium hydroxide (3 mL). About 20 mL of MeOH was removed in vacuo, the residue diluted with water (30 mL), and extracted with EtOAc (3 x 30 mL). The combined organics were washed with water (5 x 25 mL), brine (30 mL), dried (K2CO3), evaporated in vacuo and purified by column chromatography (Kieselgel 60, 230-400 mesh, CH2Cl2-MeOH 95/5 to 90/10 to 85/15) to give amine compound 39 (80 mg, 0.244 mmol, 61 %) as colorless oil.HRMS Calcdfor C22H27FN2O: 354.2107; Found: 354.2107.

With the rapid development of chemical substances, we look forward to future research findings about 23147-58-2.

Reference:
Patent; JANSSEN PHARMACEUTICA N.V.; WO2006/61392; (2006); A2;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Reference of 23783-42-8, 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. 23783-42-8, name is 2,5,8,11-Tetraoxatridecan-13-ol, molecular formula is C9H20O5, 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.

An oven-dried 100 mL round bottom flask was charged with t-BuOK (13 mmol), dry THF (30 mL), purged with argon and cooled to 0C in an ice bath. Tetraethyleneglycol monomethyl ether (10 mmol) was then added dropwise to the solution and the reaction stirred at 0C for 1 h under argon. Allyl bromide (13 mmol) was added dropwise, and the solution was warmed to R.T. and allowed to stir for 24 h under argon. Deionized water (2 mL) was then added and the reaction stirred for 10 min. All liquid were then removed in vacuo and the residue redissolved in ethyl acetate (50 mL). The organic was washed three times with water (20 mL), dried over Na2S04, filtered over Celite and then concentrated in vacuo to yield clear/light yellow oil (47%). iHNMR (400 MHz, CDCb): delta = 5.90 (m, 1H), 5.23 (dd, 1H, 3jHHtram = 17.3 Hz, , 2jHHgem = 1.7 Hz), 5.15 (dd, 1H, 3JHH = 10.4 Hz, , iJHHgem = 1.5 Hz), 4.00 (dd, 2H, SJHH = 5.89 Hz, , 4JHH = 1.5 Hz), 3.65 (m, 12H), 3.59 (m, 2H), 3.53 (m, 2H), 3.36 (s 3H) ppm. isCNMR (400 MHz, CDCb): delta =134.8, 117.0, 72.2, 71.9, 70.6, 70.6, 70.6, 70.5, 69.4, 59.0 ppm. HRMS-ESI: Calculated [M+Na]+: 271.1516; found: 271.1516.

According to the analysis of related databases, 23783-42-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; THE REGENTS OF THE UNIVERSITY OF CALIFORNIA; GARRELL, Robin L.; TUCKER-SCHWARTZ, Alexander K.; WO2012/129380; (2012); A2;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

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 3513-81-3, name is 2-Methylenepropane-1,3-diol. This compound has unique chemical properties. The synthetic route is as follows. Formula: C4H8O2

Example 7; 5-Cvclopropyl-2-(4-fluorophenyl)-6-rr(2-hvdroxy-1 ,2-oxaborolan-4- yl)methyll(methylsulfonyl)aminol-N-methyl-1 -benzofuran-3-carboxamide Step 1 : 3-chloro-2-(chloromethyl)prop-1 -eneA solution of thionyl chloride (290 g, 1 19 mmol) in DCM (200 mL) was added dropwise into a mixture of 2-methylenepropane-1 ,3-diol (88 g, 1 mol), dry pyridine (150 mL), and dry DCM (100 mL). The reaction mixture was heated to reflux with stirring for 3 hours and then allowed to stand overnight. The mixture was cooled to room temperature and poured into ice. The solution was neutralized with solid sodium bicarbonate and then extracted with diethyl ether(3 <0.6 L) followed by washing the ether extracts with dilute sulfuric acid. The combined organic layers were dried with anhydrous sodium sulfate, filtered, and concentrated in vacuo to give a residue which was fractionated to give 3-chloro-2- (chloromethyl)prop-l -ene (40.1 g, 32percent) as a colorless oil. With the rapid development of chemical substances, we look forward to future research findings about 3513-81-3. Reference:
Patent; GLAXO GROUP LIMITED; JOHNS, Brian Alvin; SHOTWELL, John Brad; HAIGH, David; WO2012/67663; (2012); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

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.647-42-7, name is 3,3,4,4,5,5,6,6,7,7,8,8,8-Tridecafluorooctan-1-ol, molecular formula is C8H5F13O, molecular weight is 364.1, as common compound, the synthetic route is as follows.Computed Properties of C8H5F13O

The same fluoroalkyloxy alkanes as in Examples 1- 4 were prepared following an alternative procedure. A mixture comprising 0.1 moles of fluorinated alcohol, 60 ml of N-methyl-2-pyrrolidone, 0.2 moles of 1- bromoalkane, and 60 ml of a 45% aqueous solution of KOH was heated under stirring for 5 hours at 500C, then at 700C for 2 hours so as to complete the reac- tion. The raw reaction mixture was filtered so as to remove the formed KBr, and then diluted in 20 ml of water; the organic phase thus obtained comprised the desired fluoroalkyloxy alkane (yield: 80%) .

At the same time, in my other blogs, there are other synthetic methods of this type of compound,647-42-7, 3,3,4,4,5,5,6,6,7,7,8,8,8-Tridecafluorooctan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; ALChiMI.A. S.r.l.; WO2009/133575; (2009); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Adding a certain compound to certain chemical reactions, such as: 372-30-5, Ethyl 4,4,4-trifluoro-3-hydroxybutyrate, 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: C6H9F3O3, blongs to alcohols-buliding-blocks compound. COA of Formula: C6H9F3O3

(1) Protection of a hydroxyl group of ethyl 4,4,4-trifruolo-3-hydroxybutyrate with dihydropyran With stirring, 7 ml of conc. hydrochloric acid was added dropwise to a mixture of 33.4 g of R-(+)-ethyl 4,4,4-trifluoro-3-hydroxybutyrate and 22.6 g of dihydropyran under ice cooling. After the dropwise addition, stirring continued at room temperature for another 5 hours. The reaction mixture was poured into ice water, neutralized with sodium hydrogen carbonate, and then extracted with methylene chloride. After drying, the solvent was evaporated. The residue was distilled under reduced pressure of 6 mmHg to obtain 41.3 g of final ethyl 4,4,4-trifluoro-3-tetrahydropyranyloxybutyrate (1) (yield 85 %).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,372-30-5, Ethyl 4,4,4-trifluoro-3-hydroxybutyrate, and friends who are interested can also refer to it.

Reference:
Patent; Mitsubishi Gas Chemical Company, Inc.; US5264150; (1993); A;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Adding a certain compound to certain chemical reactions, such as: 149104-89-2, (4-Bromo-3-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, 149104-89-2, blongs to alcohols-buliding-blocks compound. HPLC of Formula: C8H9BrO

3.7 g (43 mmol, 10 eq) of manganese dioxide are added to a solution of 900 mg (4.3 mmol, 1 eq) of (4-bromo-3-methylphenyl)methanol in 8 mL of dichloromethane. The reaction mixture is stirred for 12 hours at room temperature. The solid is filtered off and the solvent is evaporated off. 900 mg of 4-bromo-3-methylbenzaldehyde are obtained in oil form and used in the following reaction without further purification

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,149104-89-2, its application will become more common.

Reference:
Patent; GALDERMA RESEARCH & DEVELOPMENT, S.N.C.; WO2006/18326; (2006); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Adding a certain compound to certain chemical reactions, such as: 24034-73-9, (2E,6E,10E)-3,7,11,15-Tetramethylhexadeca-2,6,10,14-tetraen-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, name: (2E,6E,10E)-3,7,11,15-Tetramethylhexadeca-2,6,10,14-tetraen-1-ol, blongs to alcohols-buliding-blocks compound. name: (2E,6E,10E)-3,7,11,15-Tetramethylhexadeca-2,6,10,14-tetraen-1-ol

0441] 2E,6E,10E)-3)7,ll,15-tetramethylhexadeca-2,6,10i14-tetraen-l-yl 4- methylpiperazine-l-carboxylate (40a): To a solution of alcohol 1 (160 mg, 55 mmol) in DCM (3 mL) at 0 C was added carbonyldiimidazole (CDI) (107 mg, 0.66 mmol) and the reaction was stirred for 1 h. Then N-methylpiperazine (80 mg, 0.72 mmol) and DMAP (68 mg, 0.55 mmol) were added and stirred for 12 h. Solvent was removed and the residue was purified by column chromatography (DCM/ MeOH) to give the carbamate 40a as a viscous oil in 88 % yield (191 mg). TLC Rf: 0.54 (10% MeOH/DCM); JH NM R (300 MHz, CDCI3): delta 5.34 (t, 3H), 5.08 (m, 3H), 4.59 (d, 2H), 3.49 (m, 4H), 2.35 (m, 4H), 2.29 (s, 3H), 2.10-1.97 (m, 12H), 1.70 (s, 3H), 1.67 (s, 3H ), 1.59 (s, 9H); LCMS: MS (m/z): 417 (M+H ).

The synthetic route of 24034-73-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; COYOTE PHARMACEUTICALS, INC.; SERIZAWA, Hiroaki; ARGADE, Ankush B.; DATWANI, Akash; SPENCER, Natalie; PAN, Yonghua; ERMINI, Florian; WO2013/130654; (2013); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Reference of 764-48-7 ,Some common heterocyclic compound, 764-48-7, molecular formula is C4H8O2, 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 round bottom flask 1 L, 1,1′-thiocarbonyldiimidazole 3.6 g (20.2 mmol), 2-hydroxyethyl vinyl ether (95% purity) 1.9 mL (20.2 mmol) and toluene 60mL was added, 60 at was refluxed for 6 hours. Then allowed to cool to room temperature, potassium hydroxide 0.05g (0.89mmol) and benzyl mercaptan 2.4mL of (20.5 mmol) was added, and the mixture was refluxed for 6 hours again 60 C.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,764-48-7, its application will become more common.

Reference:
Patent; UNIVERSITYOF FUKUI; MARUZENPETROCHEMICAL COMPANY LIMITED; SUGIHARA, SHINJI; (22 pag.)JP5818142; (2015); B2;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts