Category: 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. Application In Synthesis of 1,1,1-Trifluoro-3-iodopropane

A vial was charged with activated zinc (Rieke Zinc) (4.38 ml, 3.35 mmol) and cooled to 0C. 1,1,1-trifluoro-3-iodopropane (0.268 ml, 2.233 mmol) was added slowly dropwise and the reaction was warmed to room temperature and stirred for one hour. Palladium(II) acetate (2.73 mg, 0.012 mmol), 2?-(dicyclohexylphosphino)-N2,N2,N6,N6- tetramethyl-[ 1,1 ?-biphenylj -2,6-diamine (CPhos) (10.60 mg, 0.024 mmol), and 1 -(4-bromo-5- fluoro-2-methoxyphenyl)-N-(isoxazol-3 -yl)-2-oxo- 1 ,2-dihydroquinoline-6-sulfonamide (See above Intermediate B 1, 0.100 g, 0.202 mmol) were added and the reaction was stirred for two hours at 50 C. The reaction was diluted with ethyl acetate and washed twice with iN HC1 solution. The organic layer was washed with brine, dried with sodium sulfate, filtered, and concentrated. The material was purified via column chromatography (RediSep Gold 40g, gradient elution 0-100% EtOAc :Heptane) to afford (P)- 1 -(5 -fluoro-2-methoxy-4-(3 ,3,3 – trifluoropropyl)phenyl)-N-(isoxazol-3 -yl)-2-oxo- 1 ,2-dihydroquinoline-6-sulfonamide (0.067 g, 0.131 mmol, 64.8 % yield) as a white solid. 1H NMR (400 MHz, DM50-cl6) oe = 2.64 – 2.78 (m, 2 H) 2.87-3.03 (m, 2 H) 3.66 (s, 3 H) 6.44 (d, J1.81 Hz, 1 H) 6.77 (dd, J15.32,9.30 Hz, 2 H) 7.30 – 7.41 (m, 2 H) 7.84 (dd, J=8.97, 2.23 Hz, 1 H) 8.21 (d, J=9.69 Hz, 1 H)8.36 (d, J=2.18 Hz, 1 H) 8.73 (d, J=1.76 Hz, 1 H) 11.65 (s, 1 H). m/z (ESI) 512.2 (M+H)t

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 460-37-7, its application will become more common.

Reference:
Patent; AMGEN INC.; WEISS, Matthew; MILGRAM, Benjamin C; MARX, Isaac E.; DINEEN, Thomas; (63 pag.)WO2017/106871; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, belongs to iodides-buliding-blocks compound, 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 460-37-7, category: iodides-buliding-blocks

Example 40/V-{[(2S)-5-FLUORO-7-(METHYLSULFONYL)-2,3-DIHYDRO-1 ,4-BENZODIOXIN-2- YL]METHYLJ-N-(S1S1S-TRIFLUOROPROPYL)AMINEA mixture of 1 -[(2S)-5-fluoro-7-(methylsulfonyl)-2,3-dihydro-1 ,4-benzodioxin-2- 5 yl]methaneamine (0.3 g, 1.1 mmol), 1 ,1 ,1 -trifluoro-3-iodopropane (0.16 ml, 1.4 mmol) K2CO3 (0.32 g, 2.3 mmol) and ACN (4 ml) was heated under microwave radiation at 1200C for 30 min. The mixture was filtrated and evaporated to dryness and the product was purified by flash column chromatography (EtOAc).Yield: 0.12 g, 31 %. The amine was converted to the hydrochloric acid salt and crystallized from MeOH/Et2O. M. p. 10 233C. MS m/z (rel. intensity, 70 eV) 357 (M+, 1 ), 274 (3), 127 (5), 126 (bp), 69 (3). [alpha]= -53 (MeOH).

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.

Reference:
Patent; NSAB, FILIAL AF NEUROSEARCH SWEDEN AB, SVERIGE; WO2009/133107; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 460-37-7, These common heterocyclic compound, 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, 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 solution of Zinc ((1 S,3S)-3-(methyl(7-tosyl-7H-pyrrolo[2,3-d]pyrimidin-4- yl)amino)cyclobutyl)-methanesulfinate (100 mg, 0.230 mmol) in DMSO (8 mL) was added 1 ,1 ,1 – trifluoro-3-iodopropane (1 29 mg, 0.575 mmol) and K2CO3(95.4 mg, 0.690 mmol). The solution was stirred at 50oC for 2 hours by which time LCMS showed the reaction was complete. The mixture was diluted with water (30 mL), extracted with EtOAc (30 mL x 2). The combined organ- ic layer was washed with brine (50 mL), dried over Na2SO4, filtered and concentrated. The crude product was purified by silica gel chromatography (EtOAc: PE=2:1 ) to afford the title compound (45 mg, 37%) as a colorless oil. LCMS m/z 531 .1 [M+H]+

Statistics shows that 1,1,1-Trifluoro-3-iodopropane is playing an increasingly important role. we look forward to future research findings about 460-37-7.

Reference:
Patent; PFIZER INC.; COFFMAN, Karen J.; DUERR, James M.; KAILA, Neelu; PARIKH, Mihir D.; REESE, Matthew R.; SAMAD, Tarek; SCIABOLA, Simone; TUTTLE, Jamison B.; VAZQUEZ, Michael L.; VERHOEST, Patrick Robert; (254 pag.)WO2016/24185; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application 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.

Methyl 1H-1,2,4-triazole-3-carboxylate (8.11 g, 63.8 mmol) was dissolved in DMF (41 ml) andcooled to 0C. Sodium hyride (3.32 g, 60% purity, 82.9 mmol) was added and the reaction mixturewas stirred for 30 mm at 0C. After 1,1,1-trifluoro-3-iodopropane (15.0 g, 67.0 mmol) was added the reaction mixture was stirred for 16 h at room temperature. Aqueous ammoniumchloride solution and ethyl acetate were added. Layers were separated and aqueous layer was extracted with ethyl acetate. Combined organic extracts were washed with brine, dried with sodium sulfate andsolvents were removed in vacuo. The crude product was purified by preparative HPLC (Method 4) affording 2.56 g (18% of th.) of the title compound?H-NMR (400 MHz, DMSO-d6) oe [ppm]: 2.904 (0.96), 2.921 (2.07), 2.932 (2.97), 2.938 (1.52),2.948 (5.97), 2.959 (3.22), 2.966 (3.45), 2.976 (5.83), 2.987 (1.41), 2.993 (3.06), 3.004 (1.93),3.021 (0.94), 3.331 (1.18), 4.556 (8.10), 4.573 (16.00), 4.590 (7.72), 8.776 (11.85).

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; BAYER PHARMA AKTIENGESELLSCHAFT; COLLIN-KROePELIN, Marie-Pierre; KOLKHOF, Peter; NEUBAUER, Thomas; FUeRSTNER, Chantal; POOK, Elisabeth; TINEL, Hanna; SCHMECK, Carsten; WASNAIRE, Pierre; SCHIRMER, Heiko; LUSTIG, Klemens; (131 pag.)WO2019/81306; (2019); A1;,
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. Computed Properties of C3H4F3I

To a solution of 500 mg (1.79 mmol) of the compound from Ex. 35A in 22 ml of DMF were added 620 mg (4.49 mmol) of potassium carbonate, and the mixture was stirred at RT for 15 min. Then 1.24 g (5.39 mmol) of 1,1,1-trifluoro-3-iodopropane were added, and the mixture was stirred at 50 C. for 15 h. The DMF was very substantially distilled off and the residue obtained was partitioned between semisaturated sodium chloride solution (100 ml) and ethyl acetate (50 ml). The water phase was extracted with ethyl acetate. The combined organic phases were dried over sodium sulfate, filtered and concentrated. The residue obtained was chromatographed using a silica gel cartridge (Biotage, 100 g of silica gel, eluent: hexane/ethyl acetate 94:6?50:50). In this way, 600 mg (88% of theory) of the title compound were obtained. 1H-NMR (400 MHz, DMSO-d6, delta/ppm): 10.09 (s, 1H), 4.15 (br. d, 2H), 2.85-2.71 (m, 5H), 2.42 (dd, 1H), 1.17 (s, 3H), 1.06 (dd, 1H), 0.87 (s, 3H), 0.73 (dd, 1H). LC/MS (Method 4, ESIpos): Rt=1.32 min, m/z=375 [M+H]+.

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

Electric Literature 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.

A solution of 880 mg (2.76 mmol) of the compound from Ex. 114A in 12 mL of DMF was treated with 1:35 g (4.15 mmol) cesium carbonate and stirred for 20 min at RT.Then 929 mg (4.15 mmol) 3,3,3-trifluoro-1-iodopropane were added, and the mixture was 2 h at 80 C heats.After cooling to RT was diluted with about 100 ml of ethyl acetate and washed twice with about 100 ml of water and once with 100 ml of saturated sodium chloride solution.After drying over anhydrous magnesium sulfate, was filtered and concentrated.The crude product was purified by preparative HPLC (method 6).The product fractions were combined and concentrated and the residue dried under high vacuum.There were 750 mg (63% d. Th.) Of the title compound.

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.

Electric Literature of 460-37-7, These common heterocyclic compound, 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, 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.

Example 91Preparation of Compound 496Step A – synthesis of compound 9JBCompound 91 A (5.Og, 22mol) was added to Mg turnings (0.7Og, 29mga) and catalytic iodine in ether (3OmL). After Ih, the reaction was cooled to 0 0C and treated with benzaldehyde (2.08g, 20mmol). After Ih , satd. NH4Cl was added (10OmL). The ether was concentrated to leave a yellow oil, taken up in CH2Cl2 (4OmL), and treated with PCC (12.0g, 56mmol) for 4h. Hexane (30ml) was added, the solid filtered and concentrated to give crude compound 91B as a yellow solid.

Statistics shows that 1,1,1-Trifluoro-3-iodopropane is playing an increasingly important role. we look forward to future research findings about 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. COA of Formula: C3H4F3I

General procedure: Example 20A Methyl 1-(2-methoxyethyl)-3,5-dimethyl-2,4-dioxo-1,2,3,4-tetrahydrothieno[2,3-d]pyrimidine-6-carboxylate 1.246 g (3.825 mmol) of caesium carbonate were added to a solution of 402 mg (1.25 mmol) of the compound from Ex. 18A in 12.3 ml of DMF, and the mixture was stirred at RT for 10 min. Then 452 mg (3.18 mmol) of iodomethane were added, and the mixture was stirred at RT for 22 h. The reaction mixture was then partitioned between water (75 ml) and dichloromethane (75 ml). The aqueous phase was extracted with dichloromethane. The combined organic phases were dried over sodium sulphate, filtered and concentrated. The residue obtained was chromatographed on silica gel (hexane/ethyl acetate eluent). 248 mg (59% of theory) of the title compound were obtained. 1H-NMR (400 MHz, DMSO-d6, delta/ppm): 4.47 (t, 2H), 4.14-4.06 (m, 4H), 3.65 (t, 2H), 3.24 (s, 3H), 2.86-2.73 (m, 5H), 2.65-2.54 (m, 2H) LC/MS (Method 3): Rt=1.39 min, m/z=477 [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 460-37-7, its application will become more common.

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

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. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, A new synthetic method of this compound is introduced below., Recommanded Product: 460-37-7

A solution of 2.0 g (5.95 mmol) of the compound from Ex. 21 A in 40 ml DMF was added 1.39 g (13.1 mmol) of cesium carbonate and stirred for 15 min at RT.Then 2.66 g (11.9 mmol) 3,3,3-trifluoro-1-iodopropane were added, and the mixture was heated to 60 C.After 1 hour, additional 2.66 g (11.9 mmol) 3,3,3-trifluoro-1-iodopropane added.Stirring at 60 C was continued for 16 hours.After cooling to RT was treated with about 160 ml of water supply and is extracted three times with 80 ml of diethyl ether.The combined organic extracts were washed with saturated sodium chloride solution.After drying over anhydrous magnesium sulfate, was filtered and evaporated.The crude product was purified by MPLC on a Puriflash cartridge (100 g silica gel, cyclohexane / ethyl acetate 7: 1-> 1: 1).The product fractions were combined, evaporated and the residue dried under high vacuum.There were 1.86 g (72% d. Th.) Of the title compound.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; HAERTER, MICHAEL; DELBECK, MARTINA; KALTHOF, BERND; LUSTIG, KLEMENS; LINDNER, NIELS; KAST, RAIMUND; WASNAIRE, PIERRE; SUESSMEIER, FRANK; (372 pag.)TW2016/7950; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, A new synthetic method of this compound is introduced below., SDS of cas: 460-37-7

General procedure: 500 mg (2.00 mmol) of the compound from Ex. 31A and 690 mg (5.00 mmol) of potassium carbonate were stirred in 10 ml of anhydrous DMF at RT for 15 min, before 449 mul (4.00 mmol) of (bromomethyl)cyclobutane were added. Then the reaction mixture was stirred at 50 C. for about 16 h. After cooling to RT, water was added and the mixture was extracted with ethyl acetate. The organic extract was washed with saturated sodium chloride solution, dried over anhydrous magnesium sulfate, filtered and concentrated. The product was isolated by means of MPLC (Biotage Isolera One, SNAP KP-Sil cartridge, 50 g of silica gel, eluent: cyclohexane/ethyl acetate 2:1). After concentration of the product fractions and drying under high vacuum, 486 mg (76% of theory) of the title compound were obtained. 1H-NMR (400 MHz, DMSO-d6, delta/ppm): 10.07 (s, 1H), 3.96 (d, 2H), 2.82-2.69 (m, 1H), 2.76 (s, 3H), 2.66-2.58 (m, 1H), 2.04-1.91 (m, 2H), 1.89-1.74 (m, 4H), 1.07-0.96 (m, 2H), 0.73-0.64 (m, 2H). LC/MS (Method 1, ESIpos): Rt=1.89 min, m/z=319.11 [M+H]+.

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

Reference:
Patent; Bayer Aktiengesellschaft; Bayer Pharma Aktiengesellschaft; HAERTER, Michael; KOSEMUND, Dirk; CANCHO GRANDE, Yolanda; DELBECK, Martina; KALTHOF, Bernd; LUSTIG, Klemens; SUESSMEIER, Frank; US2020/16159; (2020); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com