Category: 431-47-0

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. 431-47-0, name is Methyl 2,2,2-trifluoroacetate, A new synthetic method of this compound is introduced below., Safety of Methyl 2,2,2-trifluoroacetate

Synthesis Example 40 Synthesis of N-propargyltrifluoroacetamide Propargylamine (Aldrich, 25 g, 0.45 mol) was added dropwise to methyl trifluoroacetate (Tokyo Chemical Industry Co., Ltd., 69.2 g, 0.54 mol) cooled to 0 C. They were allowed to react at 0 C. for two hours to afford 43.8 g (86.0%) of N-propargyltrifluoroacetamide after purification by vacuum distillation (23 mmHg, boiling point; 77 C.).

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; The Institute of Physical and Chemical Research; US6365350; (2002); B1;,
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Adding a certain compound to certain chemical reactions, such as: 431-47-0, name is Methyl 2,2,2-trifluoroacetate, belongs to esters-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 431-47-0, Formula: C3H3F3O2

4-bromo-1-(secbutyl)-1H-pyrazole (1.0 g, 5.0 mmol) was dissolved in dry THF (15 mL) at -78 C under nitrogen and was stirred for 10min. n-BuLi (2.5 M in hexanes, 2.1 mL, 5.2 mmol) was added drop wise to the solution was stirred for 2 h at -78 C. After two hours, methyl trifluoroacetate (0.85 mL, 8.5 mmol) was added drop wise and stirred for 30 min at -78 C. The solution was then allowed to warm up to room temperature and let stir for overnight. The mixture was then quenched with NH4Cl (20mL) and extracted with ether (50 mL), and dried over MgSO4. After concentration in vacuo(note: remove shortly after the ether is removed, because the compound is quite volatile), the residue was purified with flash chromatography over silica gel (hexane: ether = 98:2) to yield the product as a liquid.

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, Methyl 2,2,2-trifluoroacetate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Camerino, Eugene; Wong, Dawn M.; Tong, Fan; Koerber, Florian; Gross, Aaron D.; Islam, Rafique; Viayna, Elisabet; Mutunga, James M.; Li, Jianyong; Totrov, Maxim M.; Bloomquist, Jeffrey R.; Carlier, Paul R.; Bioorganic and Medicinal Chemistry Letters; vol. 25; 20; (2015); p. 4405 – 4411;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 431-47-0 as follows. Formula: C3H3F3O2

A. Preparation of N-propargyltrifluoroacetamide (43) Propargylamine (24.79 g, 0.450 mole; Aldrich, 99%) was added dropwise over 1 h to methyl trifluoroacetate (69.19 g, 0.540 mole, 1.2 eq, Aldrich) at 0. After stirring an additional hour at 0, distillation though a 15 cm Vigreux column afforded 62.12 g (91%) of trifluoroacetamide 43 as a colorless liquid (bp 68.5-69.5 at 11 torr). This material was homogeneous by NMR and GC and was used interchangeably with spectroscopically-identical material prepared by acylating propargylamine with trifluoroacetic acid anhydride. 1 H-NMR (CDCl3): 6.85 (broad s, 1H, NHTFA), 4.17 (dd, J=5.6 and 2.5, 2H, CH2), 2.35 (t, J=2.5, 1H, CH). IR (neat; cm-1): 3300 (N–H), 3095 and 2935 (C–H), 2130 (acetylene), 1720 (C=O), 1550 (N–H), 1430, 1365, 1160, 1040, 998, 918, 857, 829, 772, and 725.

According to the analysis of related databases, 431-47-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; E. I. Du Pont de Nemours and Company; US5151507; (1992); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Application of 431-47-0, 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. 431-47-0 name is Methyl 2,2,2-trifluoroacetate, This 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.

e) 2,2,2-Trifluoro-N-prop-2-ynyl-acetamide To 15 g (272.3 mmol) propargylamine in 275 ml anhydrous methanol 36.6 g (285.9 mmol) methyl trifluoroacetate were added with cooling. The resulting reaction mixture was stirred for an additional four hours at room temperature. Afterwards the solvent was removed by distillation at reduced pressure. The residue was dissolved in 300 ml trichloromethane and extracted four times, twice each with 300 ml of a saturated sodium bicarbonate solution and twice each with 300 ml water. The separated organic phase was dried over magnesium sulfate, filtrated and the solvent was removed by distillation (yield: 23.3 g).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl 2,2,2-trifluoroacetate, and friends who are interested can also refer to it.

Reference:
Patent; Roche Diagnostics GmbH; F.HOFFMANN-LA ROCHE AG; EP1842923; (2007); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Reference of 431-47-0, These common heterocyclic compound, 431-47-0, name is Methyl 2,2,2-trifluoroacetate, 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.

Phthalimide (100 mg, 0.68 mmol), DMSO (10 mL), CH3ONa (112 mg, 2 mmol, 3 eq.) was added to the reaction flask in turn, stirred at room temperature for 5 minutes, and then uniformly dispersed after NaH. Methyl trifluoroacetate (0.28 mL, 2.7 mmol, 4 eq.) was slowly injected into the reaction flask. After reacting for 10 hours, the TLC was plated, and the starting point disappeared, that is, the reaction was completed, and the stirring was stopped. Extract twice with ethyl acetate and distilled water, then wash with saturated NaCl solution. The organic phases were combined, and the organic phase was dried over anhydrous magnesium sulfate. The magnesium sulfate was removed by filtration, and the solvent was evaporated. Purification by column chromatography gave white solid N-methylphthalimide (109 mg,Yield 100%).

The synthetic route of 431-47-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Guangdong Petrochemical College; Xiao Duoduo; Zheng Xin; Zeng Jiechun; Huang Jiawei; Zhou Rujin; Guan Ying; Liang Jieling; (8 pag.)CN109369506; (2019); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Application of 431-47-0, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 431-47-0 as follows.

Example 58 Preparation of 1-(3,4-dichloro-5-methylphenyl)-2,2,2-trifluoroethan-1-one (C201) To 5-bromo-1,2-dichloro-3-methylbenzene (6.9 g, 29 mmol) in tetrahydrofuran (65 mL) cooled in an ice bath under nitrogen was added isopropylmagnesium chloride lithium chloride complex in tetrahydrofuran (26.8 mL, 34.8 mmol). After 1 hour methyl 2,2,2-trifluoroacetate (3.79 mL, 37.7 mmol) was added. After 30 minutes, the ice bath was removed, and the solution was stirred for 1 hour. The reaction mixture was quenched with aqueous hydrochloric acid (2 N). The mixture was concentrated and extracted with dichloromethane. The organic layer was washed with brine, dried over sodium sulfate, filtered, and concentrated. Purification by column chromatography (SiO2, petroleum ether) provided the title compound as a white solid (5.9 g, 80%): 1H NMR (400 MHz, CDCl3) delta 8.00 (s, 1H), delta 7.83 (s, 1H), 2.51 (s, 3H); EIMS m/z 256 ([M]+).

According to the analysis of related databases, 431-47-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Dow AgroSciences LLC; Barton, Thomas; Gao, Xin; Hunter, Jim; LePlae, JR., Paul R.; Lo, William C.; Boruwa, Joshodeep; Tangirala, Raghuram; Watson, Gerald B.; Herbert, John; (261 pag.)US2017/208803; (2017); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 431-47-0, name is Methyl 2,2,2-trifluoroacetate, belongs to esters-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 431-47-0, Application In Synthesis of Methyl 2,2,2-trifluoroacetate

N-benzyl p-toluenesulfonamide (100 mg, 0.38 mmol), DMF (4 mL), potassium t-butoxide (129 mg, 1.15 mmol, 3 eq.) was added to the reaction flask in turn, and stirred at room temperature for 5 minutes. After the potassium tert-butoxide was uniformly dispersed, methyl trifluoroacetate (0.15 mL, 1.52 mmol, 4 eq.) was slowly injected into the reaction flask, and after 10 hours of reaction, stirring was stopped. It was extracted twice with ethyl acetate and distilled water, and then washed with a saturated NaCI solution. The magnesium sulfate was removed by filtration, and the solvent was evaporated. Purification by column chromatography to give N-methyl-N-benzyl-p-toluenesulfonamide (104 mg, yield 100%)

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; Guangdong Petrochemical College; Xiao Duoduo; Zheng Xin; Zeng Jiechun; Huang Jiawei; Zhou Rujin; Guan Ying; Liang Jieling; (8 pag.)CN109369506; (2019); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Some common heterocyclic compound, 431-47-0, name is Methyl 2,2,2-trifluoroacetate, molecular formula is C3H3F3O2, 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. Recommanded Product: 431-47-0

General procedure: Amixture of carbazole 5-h (0.68 mmol) and THF (15 ml)was stirred and treated by the addition of LiH (0.03 g,3.40 mmol) and methyl trifluoroacetate (0.26 g,2.03 mmol). The reaction mixture was stirred for 1.5-5 h at63, evaporated, and treated with cold 5% hydrochloricacid solution (20 ml). The precipitate was filtered off,washed with water, and then dried over P2O5.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 431-47-0, its application will become more common.

Reference:
Article; Pugachov, Dmitriy E.; Kostryukova, Tatiana S.; Zatonsky, Georgy V.; Vatsadze, Sergey Z.; Vasil?ev, Nikolai V.; Chemistry of Heterocyclic Compounds; vol. 54; 5; (2018); p. 528 – 534; Khim. Geterotsikl. Soedin.; vol. 54; 5; (2018); p. 528 – 534,7;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics