A new synthetic route of 1228631-54-6

At the same time, in my other blogs, there are other synthetic methods of this type of compound,1228631-54-6, 1-(6-(Trifluoromethyl)pyridin-3-yl)ethanol, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 1228631-54-6, 1-(6-(Trifluoromethyl)pyridin-3-yl)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, Safety of 1-(6-(Trifluoromethyl)pyridin-3-yl)ethanol, blongs to pyridine-derivatives compound. Safety of 1-(6-(Trifluoromethyl)pyridin-3-yl)ethanol

To a 0 C mixture l-(6-(trifluoromethyl)pyridin-3-yl)ethanol (8.0 mmol) and triphenylphosphine (3.8 g, 14.6 mmol) in THF (55 mL) under N2atmosphere is added perbromomethane (3.8 g,12.2 mmol). After stirring at 0 C for 2 min, the mixture is allowed to warm to room temperature and stirred for 25 min. The precipitate is filtered off through a pad of celite, the solid is washed with cold THF (10 mL). The solution is collected and organic phases combined. The solvent is removed under reduced pressure

At the same time, in my other blogs, there are other synthetic methods of this type of compound,1228631-54-6, 1-(6-(Trifluoromethyl)pyridin-3-yl)ethanol, and friends who are interested can also refer to it.

Reference:
Patent; SOLVAY SA; BRAUN, Max Josef; (21 pag.)WO2017/198812; (2017); A2;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

The origin of a common compound about 1228631-54-6

According to the analysis of related databases, 1228631-54-6, the application of this compound in the production field has become more and more popular.

Reference of 1228631-54-6, 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. 1228631-54-6, name is 1-(6-(Trifluoromethyl)pyridin-3-yl)ethanol, molecular formula is C8H8F3NO, 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.

Example 69: Preparation of Carbamates – General Method AThe acyl azide was suspended in dry toluene (0.35 M). To the resulting slurry was added the appropriate alcohol (1.20 equiv). The slurry was heated to 100 0C (external) for 4-24 h and then cooled to ambient temperature. The product was isolated by vacuum filtration or purified by silica gel column chromatography (after applying the material directly to the column) eluting with EtOAc/hexanes gradient. In some instances, further purification by recrystallization was necessary. Typical solvents used include: chloroform-Patent; DOW AGROSCIENCES LLC; LAMBERT, William; CROUSE, Gary; SPARKS, Thomas; CUDWORTH, Denise; WO2011/17513; (2011); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Brief introduction of 1-(6-(Trifluoromethyl)pyridin-3-yl)ethanol

According to the analysis of related databases, 1228631-54-6, the application of this compound in the production field has become more and more popular.

Related Products of 1228631-54-6, 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. 1228631-54-6, name is 1-(6-(Trifluoromethyl)pyridin-3-yl)ethanol, molecular formula is C8H8F3NO, 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.

Example 74: Preparation of O-l-(6-(trifluoromethyl)pyridin-3-yl)ethyl 4-(l-(4-(trifluoromethoxy)phenyl)-lH-l,2,4-triazol-3-yl)phenylcarbamothioate (Compound 133)Under a N2 atmosphere, thiophosgene (0.56 mmol) was added dropwise to cold dichloromethane cooled in an ice bath. To this solution was added a cold 0.2 mM (0.13 mmol) K2CO3 solution. The reaction was stirred for 10 min. 4-(l-(4- (Trifluoromethoxy)phenyl)-lH-l,2,4-triazol-3-yl)aniline (0.56 mmol) was dissolved in dichloromethane and added dropwise to the above mixture. The reaction was allowed to stir for another 10 min. A cold 0.6 mM (0.92 mmol) KOEta solution was then added. After 30 min, the reaction mixture was diluted with dichloromethane and washed with water and brine. The organic layer was dried over MgSO4 and concentrated. The crude isothiocyanate was used without further purification in the next step.To a slurry of NaH (9.2 mg of a 60% suspension in mineral oil, 0.229 mmol) in THF (1 mL) at 0 0C was added l-(6-(trifluoromethyl)pyridine-3-yl)ethanol (43.7 mg, 0.229 mmol) in PhCH3 (0.4 mL). The mixture was warmed to ambient temperatue and stirred for 15 min, and then the isothiocyanate from above (75.6 mg, 0.209 mmol) in THF (1 mL) was added via cannula. After stirring for 20 min, the mixture was quenched by addition of aq NH4Cl solution and extracted with EtOAc (x3). The combined organic extracts were washed with brine, dried over Na2SO4, and concentrated. The crude product was applied to a silica gel column, and elution with a 15% to 40% to 65% EtOAc/hexanes gradient provided the title compound (88.2 mg, 77%) as an off-white solid: mp 186.5-188 0C; 1H NMR (300 MHz, CDCl3) delta 8.76 (s, IH), 8.58 (s, IH), 8.50 (s, IH), 8.19 (d, J= 8.7 Hz, 2H), 7.91-7.83 (m, IH), 7.80 (d, J = 9.1 Hz, 2H), 7.69 (d, J = 8.1 Hz, IH), 7.49-7.29 (m, 4H), 6.68 (q, J = 6.7 Hz, IH), 1.76 (d, J= 6.6 Hz, 3H); HRMS-FAB (m/z) [M+H]+ calcd for C24Hi7F6N5O2S, 553.101; found, 553.1006.

According to the analysis of related databases, 1228631-54-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; DOW AGROSCIENCES LLC; LAMBERT, William; CROUSE, Gary; SPARKS, Thomas; CUDWORTH, Denise; WO2011/17513; (2011); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Brief introduction of 1-(6-(Trifluoromethyl)pyridin-3-yl)ethanol

According to the analysis of related databases, 1228631-54-6, the application of this compound in the production field has become more and more popular.

Related Products of 1228631-54-6, 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. 1228631-54-6, name is 1-(6-(Trifluoromethyl)pyridin-3-yl)ethanol, molecular formula is C8H8F3NO, 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.

Example 74: Preparation of O-l-(6-(trifluoromethyl)pyridin-3-yl)ethyl 4-(l-(4-(trifluoromethoxy)phenyl)-lH-l,2,4-triazol-3-yl)phenylcarbamothioate (Compound 133)Under a N2 atmosphere, thiophosgene (0.56 mmol) was added dropwise to cold dichloromethane cooled in an ice bath. To this solution was added a cold 0.2 mM (0.13 mmol) K2CO3 solution. The reaction was stirred for 10 min. 4-(l-(4- (Trifluoromethoxy)phenyl)-lH-l,2,4-triazol-3-yl)aniline (0.56 mmol) was dissolved in dichloromethane and added dropwise to the above mixture. The reaction was allowed to stir for another 10 min. A cold 0.6 mM (0.92 mmol) KOEta solution was then added. After 30 min, the reaction mixture was diluted with dichloromethane and washed with water and brine. The organic layer was dried over MgSO4 and concentrated. The crude isothiocyanate was used without further purification in the next step.To a slurry of NaH (9.2 mg of a 60% suspension in mineral oil, 0.229 mmol) in THF (1 mL) at 0 0C was added l-(6-(trifluoromethyl)pyridine-3-yl)ethanol (43.7 mg, 0.229 mmol) in PhCH3 (0.4 mL). The mixture was warmed to ambient temperatue and stirred for 15 min, and then the isothiocyanate from above (75.6 mg, 0.209 mmol) in THF (1 mL) was added via cannula. After stirring for 20 min, the mixture was quenched by addition of aq NH4Cl solution and extracted with EtOAc (x3). The combined organic extracts were washed with brine, dried over Na2SO4, and concentrated. The crude product was applied to a silica gel column, and elution with a 15% to 40% to 65% EtOAc/hexanes gradient provided the title compound (88.2 mg, 77%) as an off-white solid: mp 186.5-188 0C; 1H NMR (300 MHz, CDCl3) delta 8.76 (s, IH), 8.58 (s, IH), 8.50 (s, IH), 8.19 (d, J= 8.7 Hz, 2H), 7.91-7.83 (m, IH), 7.80 (d, J = 9.1 Hz, 2H), 7.69 (d, J = 8.1 Hz, IH), 7.49-7.29 (m, 4H), 6.68 (q, J = 6.7 Hz, IH), 1.76 (d, J= 6.6 Hz, 3H); HRMS-FAB (m/z) [M+H]+ calcd for C24Hi7F6N5O2S, 553.101; found, 553.1006.

According to the analysis of related databases, 1228631-54-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; DOW AGROSCIENCES LLC; LAMBERT, William; CROUSE, Gary; SPARKS, Thomas; CUDWORTH, Denise; WO2011/17513; (2011); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem