Category: 460-37-7

Application of 460-37-7, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Fluorene (6.64 g, 40 mmol) was dissolved in 27 mL of THF. After replacing the atmosphere in a reaction vessel with a nitrogen gas, the solution thus obtained was cooled to -20 C. After adding dropwise 15.8 g of n-butyllithium (1.6 M hexane solution) in a reaction vessel, the temperature of the reaction solution was returned to room temperature. Then, the reaction solution was stirred for one hour. The reaction solution was cooled to -78 C. and 8.96 g (80 mmol) of 1-iodo-3,3,3-trifluoropropane was gradually added. The mixture thus obtained was reacted by stirring for one hour after heating to room temperature. After the reaction, 90% acetic acid was added to the mixture, and then a saturated saline solution and hexane were added. The mixed solution thus obtained was separated into the organic layer and the aqueous layer. After the organic layer thus obtained was dehydrated over anhydrous sodium sulfate, the solvent was removed from the organic layer using a rotary evaporator to obtain 6.45 g (yield: 45%) of 9,9-di-3,3,3-trifluoro-n-propylfluorene.

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, 1,1,1-Trifluoro-3-iodopropane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; TOKYO OHKA KOGYO CO., LTD.; TADOKORO, Yoshinori; SHIOTA, Dai; (43 pag.)US2017/160636; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 460-37-7, A common heterocyclic compound, 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, molecular formula is C3H4F3I, 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.

Method A: 1.8 g (7.13 mmol) of the compound from Ex. 49A and 3.49 g (10.7 mmol) of caesium carbonate were stirred in 15 ml of DMF at RT for 10 min, before 1.3 ml (10.7 mmol) of 1,1,1-trifluoro-3-iodopropane were added. Subsequently, the reaction mixture was stirred at a temperature of 100 C. in a microwave oven (Biotage Initiator with dynamic control of irradiation power). After 2 h, a further 167 mul (1.43 mmol) of 1,1,1-trifluoro-3-iodopropane were added and the heating was continued for 30 min. After cooling to RT, the mixture was diluted with about 75 ml of ethyl acetate and washed successively with water and saturated sodium chloride solution. After drying over anhydrous magnesium sulphate, the mixture was filtered and the filtrate was evaporated to dryness. The crude product was purified by MPLC (Biotage cartridge, 100 g of SNAP KP-Sil silica gel, eluent: cyclohexane/ethyl acetate 1:2). After concentration and drying, a mixture of N- and O-alkylated product was obtained, from which it was possible to obtain the N-alkylated main product in solid form by stirring with a mixture of 30 ml of pentane and 2 ml of dichloromethane. Further N-alkylated product was obtained from the concentrated mother liquor from the stirring by means of preparative HPLC (Method 8). After concentration of the product fractions and drying under high vacuum, together with the solids from the stirring, 1.86 g (74% of theory) of the title compound were obtained.

The synthetic route of 460-37-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; HAeRTER, Michael; KOSEMUND, Dirk; DELBECK, Martina; KALTHOF, Bernd; WASNAIRE, Pierre; SUessMEIER, Frank; LUSTIG, Klemens; (369 pag.)US2018/65981; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 460-37-7, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

6-Ch[oro-N-(piperidin-4-y[)pyrazine-2-carboxamide trifluoroacetic acid salt[Intermediate 65] (1 .49 g, 6.20 mmol, 1 .0 eq), and potassium carbonate (4.28 g, 31.0 mmol, 5.0 eq) were suspended in 33 mL acetonitrile. Then, 1,1,1- trifluoro-3-iodopropane [CAS RN: 460-37-7] (2.08 g, 9.30 mmol, 1.5 eq) was added and the reaction mixture was heated to 70C for 4 h. On cooling, the reaction mixture was diluted with water and extracted withdichloromethane/isopropanol (4/1) (2x). The combined organic phases were washed with brine. Phase separation was conducted by the use of a Whatman filter. The volatile components were removed in vacuo and the crude material was purified via preparative MPLC (Biotage Isolera; 50 g SNAP cartridge:dichloromethane -> dichloromethane/ethanol 95/5) to give 900 mg (41% yield oftheory) of the title compound.UPLC-MS (Method 1): R = 0.56 mm; MS (ESI0): m/z = 337 [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, 1,1,1-Trifluoro-3-iodopropane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; BAeRFACKER, Lars; SIEMEISTER, Gerhard; HEINRICH, Tobias; PRECHTL, Stefan; STOeCKIGT, Detlef; ROTTMANN, Antje; WO2015/113927; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 460-37-7, The chemical industry reduces the impact on the environment during synthesis 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, I believe this compound will play a more active role in future production and life.

5-Ch[oro-N-(piperidin-4-y[)pyrazine-2-carboxamide trifluoroacetic acid salt[Intermediate 68] (722 mg, 3.00 mmol, 1 .0 eq), and potassium carbonate (2.07 g, 15.0 mmol, 5.0 eq) were suspended in 33 mL acetonitrile. Then, 1,1,1- trifluoro-3-iodopropane [CAS RN: 460-37-7] (1.01 g, 4.50 mmol, 1.5 eq) was added and the reaction mixture was heated to 70C for 4 h. On cooling, the reaction mixture was diluted with water and extracted withdichloromethane/isopropanol (4/1) (2x). The combined organic phases were washed with brine. Phase separation was conducted by the use of a Whatman filter. The volatile components were removed in vacuo and the crude material was purified via preparative MPLC (Biotage Isolera; 50 g SNAP cartridge:dichloromethane -> dichloromethane/ethanol 95/5) to give 900 mg (41% yield oftheory) of the title compound.UPLC-MS (Method 1): R = 0.58 mm; MS (ESI0): m/z = 337 [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, 1,1,1-Trifluoro-3-iodopropane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; BAeRFACKER, Lars; SIEMEISTER, Gerhard; HEINRICH, Tobias; PRECHTL, Stefan; STOeCKIGT, Detlef; ROTTMANN, Antje; WO2015/113927; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 1,1,1-Trifluoro-3-iodopropane

At room temperature, 190 g (1.4 mol) of potassium carbonate was weighed into 3 L of a three-necked flask and 500 g of DMF was added,100 g (0.7 mol) of compound 16 was added and stirring was started,20-25 C was added dropwise with 205 g (0.916 mol) of trifluoroproponium chloride, After the addition of stirring for 4.5h, the TLC reaction was completed. Add 1.6kg of methanol, stir for 30min,Suction filter. The filter cake was washed twice with methanol twice. Decompression steamed filtrate to no liquid,To the residue was added 1.5 kg of water, and 1N hydrochloric acid solution was added thereto to adjust the pH to 7,Ice bath 0 ~ 3 stirring 3h, filter, 45 drying to get 137g product, the yield of 81.8%Purity HPLC: 98.5%.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 460-37-7.

Reference:
Patent; Beijing Guangbo Desai Pharmaceutical Technology Development Co., Ltd.; Yitai (Beijing) Pharmatech Co., Ltd.; Wu, Yuan; Tian, Hua; (14 pag.)CN106008633; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 460-37-7,Some common heterocyclic compound, 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, molecular formula is C3H4F3I, 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.

K2CO3 (1.313 g, 9.50 mmol) was added to a solution of 2-chloro-4-[(3£)-3- pyrrolidinylamino]benzonitrile (0.7 g, 3.17 mmol) in MeCN (20 mL) and the reaction was heated to 55 0C. l,l,l-Trifluoro-3-iodopropane (2.84 g, 12.67 mmol) was added dropwise and the reaction mixture was stirred for 24 h. After cooling, saturated NaHCOs was added and the reaction was extracted with EtOAc. The organic layer was dried over MgSO4 and concentrated to yield the product (0.72 g, 72%). LC-MS (ES) m/e 318.2 [M + H]+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,1,1-Trifluoro-3-iodopropane, its application will become more common.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2007/65093; (2007); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 1,1,1-Trifluoro-3-iodopropane

Example 299A 3-(2-Methoxy-2-methylpropyl)-5-methyl-2,4-dioxo-1-(3,3,3-trifluoropropyl)-1,2,3,4-tetrahydrothieno[2,3-d]pyrimidine-6-carbaldehyde 498 mg (3.6 mmol) of potassium carbonate were added to a solution of 450 mg (1.44 mmol) of the compound from Ex. 288A in 15 ml of DMF, and the mixture was stirred at RT for 15 min. Then 969 mg (4.32 mmol) of 1,1,1-trifluoro-3-iodopropane were added, and the mixture was stirred at 50 C. for 18 h. The DMF was then very substantially distilled off and the remaining residue was partitioned between semisaturated sodium chloride solution (100 ml) and ethyl acetate (50 ml). The aqueous phase was extracted with ethyl acetate. The combined organic phases were dried over sodium sulphate, filtered and concentrated. The residue obtained was chromatographed using a silica gel cartridge (Biotage, 50 g of silica gel, eluent: hexane/ethyl acetate). 463 mg (79% of theory) of the title compound were obtained. 1H-NMR (400 MHz, DMSO-d6, delta/ppm): 10.11 (s, 1H), 4.17 (t, 2H), 4.00 (br. s, 2H), 3.15 (s, 3H), 2.86-2.71 (m, 5H), 1.09 (s, 6H). LC/MS (Method 3, ESIpos): Rt=1.22 min, m/z=361 [M+H-CH3OH]+.

According to the analysis of related databases, 460-37-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; HAeRTER, Michael; KOSEMUND, Dirk; DELBECK, Martina; KALTHOF, Bernd; WASNAIRE, Pierre; SUessMEIER, Frank; LUSTIG, Klemens; (369 pag.)US2018/65981; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C3H4F3I

A 50-mL round bottom flask was charged with S-(3-((3-chloro-1-(pyridin-3-yl)-1H-pyrazol-4-yl)(ethyl)amino)-3-oxopropyl) ethanethioate (1.6 g, 4.54 mmol) and methanol (30 mL) The mixture was purged with a flow of nitrogen for 15 min. Sodium methoxide (0.735 g, 13.6 mmol) was added, and the suspension was stirred under nitrogen for 5 min. 1,1,1-Trifluoro-3-iodopropane (1.6 mL, 13 6 mmol) was added and the reaction was heated at 50 C. for 4 h, at which time HPLC analysis revealed complete conversion of S-(3-((3-chloro-1-(pyridin-3-yl)-1H-pyrazol-4-yl)(ethyl)amino)-3-oxopropyl) ethanethioate to product. The reaction was cooled to room temperature and transferred to a separatory funnel and EtOAc (100 mL) and water (50 mL) were added. The layers were separated and the aqueous phase was extracted with EtOAc (50 mL) The combined organic layers were washed with brine (25 mL), dried over anhydrous Na2SO4, and concentrated under reduced pressure. The residue was purified by flash column chromatography (20-100% EtOAc/hexanes) to afford an oil which solidified to give the desired product as a white solid (1.52 g, 82% yield, 97% HPLC purity). mp 79-80 C. 1H NMR (400 MHz, CDCl3): 8.94 (s, 1H), 8.62 (d, J=4.6 Hz, 1H), 8.04(d, J=9.3 Hz, 1H), 7.97 (s, 1H), 7.45 (m, 1H), 3.70 (q, J=7.0 Hz, 2H), 2.83 (t, J=7.2 Hz, 2H), 2.70-2.57 (m, 2H), 2.43 (t, J=7.2 Hz, 2H), 2.40-2.27 (m, 2H), 1.15 (t, J=7.1 Hz, 3H). ESIMS m/z 406.9 ([M+H]+).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 460-37-7.

Reference:
Patent; Dow AgroSciences LLC; YANG, Qiang; LORSBACH, Beth; NIYAZ, Noormohamed M.; BUYSSE, Ann M.; WALSH, Martin J.; Zhang, Yu; TRULLINGER, Tony K.; MOLITOR, Erich J.; CANTURK, Belgin; HAO, Yan; KISTER, Jeremy; (23 pag.)US2018/186753; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C3H4F3I

To a stirred solution of methyl 2-(3-((4-((2-methylquinolin-4-yl)methoxy)phenyl)sulfonamido)azetidin-3-yl)acetate (250 mg, 0.44 mmol) in DMF (2.50 mL), were added 1-iodo-3,3,3-trifluoropropane (51.44 mul, 0.44 mmol) and N,N-diisopropylethylamine (0.09 mL, 0.53 mmol). The reaction mixture was stirred at room temperature for 24 h. The reaction was incomplete and two further additions of 1-iodo-3,3,3-trifluoropropane (20.59 mul, 0.18 mmol) were added and the reaction mixture was left to stir over 48 h necessary to complete the reaction. The reaction mixture was diluted in EtOAc (15 mL) and the organic phase was retained, dried over MgSO4 and concentrated to dryness. The residue was dissolved in MeOH, absorbed onto silica gel and purified by flash chromatography (silica gel, 0-2% MeOH in DCM) to afford methyl 2-(3-((4-((2-methylquinolin-4-yl)methoxy)phenyl)sulfonamido)-1-(3,3,3-trifluoropropyl)azetidin-3-yl)acetate (100 mg, 41%) as a white solid.MS(ES+) m/z 552 (MH+).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 460-37-7.

Reference:
Article; Boiteau, Jean-Guy; Ouvry, Gilles; Arlabosse, Jean-Marie; Astri, Stephanie; Beillard, Audrey; Bhurruth-Alcor, Yushma; Bonnary, Laetitia; Bouix-Peter, Claire; Bouquet, Karine; Bourotte, Marilyne; Cardinaud, Isabelle; Comino, Catherine; Deprez, Benoit; Duvert, Denis; Feret, Angelique; Hacini-Rachinel, Feriel; Harris, Craig S.; Luzy, Anne-Pascale; Mathieu, Arnaud; Millois, Corinne; Orsini, Nicolas; Pascau, Jonathan; Pinto, Artur; Piwnica, David; Polge, Gaelle; Reitz, Arnaud; Reverse, Kevin; Rodeville, Nicolas; Rossio, Patricia; Spiesse, Delphine; Tabet, Samuel; Taquet, Nathalie; Tomas, Loic; Vial, Emmanuel; Hennequin, Laurent F.; Bioorganic and Medicinal Chemistry; vol. 26; 4; (2018); p. 945 – 956;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. name: 1,1,1-Trifluoro-3-iodopropane

Example 25 (rac)-cis-9-(Phenylethynyl)-4-(3,3,3-trifluoropropyl)-3,4,4a,5,6,10b-hexahydro-2H-[1,4]oxazino[2,3-f]quinoline A mixture of cis-9-(phenylethynyl)-3,4,4a,5,6,10b-hexahydro-2H-[1,4]oxazino[2,3-f]quinoline (200 mg, 0.69 mmol), 1,1,1-trifluoro-3-iodopropane (202 mg, 0.90 mmol), and NaHCO3 (126 mg, 1.50 mmol) in DMF (3 mL) is stirred at 50-60 C for 6 hours. Then an additional amount of 1,1,1-trifluoro-3-iodopropane (100 mg, 0.45 mmol) is added, and the mixture is stirred at the same temperature for 16 h, cooled down to rt, diluted with water (50 mL) and extracted with EtOAc (2*50 mL). The combined organic layers are dried over Na2SO4 and concentrated at reduced pressure. The obtained residue is purified by column chromatography (silica gel, EtOAc/hexane, 1:2) to provide the title compound (75 mg, 28%) as a yellowish oil. 1H NMR (DMSO-d6), deltaH, 1.75-1.84 (m, 1H), 2.12-2.23 (m, 1H), 2.40-2.54 (m, 3H), 2.61-2.89 (m, 4H), 2.91-3.01 (m, 2H), 3.58-3.71 (m, 2H), 4.64 (d, 1H), 7.43-7.49 (m, 3H), 7.56-7.62 (m, 2H), 7.84 (d, 1H), 8.58 (d, 1H). LC/MS (M+H)+ = 387

The synthetic route of 460-37-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Merz Pharma GmbH & Co. KGaA; The designation of the inventor has not yet been filed; EP2650284; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com