Tag: M.W=100-200

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. 18830-44-9, name is Methyl 3,3,3-trifluoropropanoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C4H5F3O2

Put 67.1g of sodium hydroxide and 300g of deionized water into a 500ml reaction bottle, cool the ice water bath to 5 10 , drop 216.6g of methyl trifluoropropionate above, control the internal temperature below 30 , and continue stirring after the dripping 30min.Concentrated hydrochloric acid was added dropwise to the reaction bottle until the pH of the reaction solution was below 2, and stirring was continued for 30 min after completion of the drop.300 g of dichloromethane was added to the reaction flask for extraction twice, and the dichloromethane was concentrated and recovered to obtain crude trifluoropropionic acid.Set up a vacuum distillation device, vacuum distillate crude trifluoropropionic acid, collect 83 ~ 85 fraction (vacuum degree -0.097MPa), which is 3,3,3-trifluoropropionic acid, weight 199g, purity 99.2%, yield 88.0%, total reaction yield 66.2%.

The synthetic route of 18830-44-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hunan Youse Chenzhoufu Chemical Co., Ltd.; Wang Gang; Peng Zhimin; Li Zhipeng; Yin Demei; Zhang Zhenhua; (8 pag.)CN110903183; (2020); A;,
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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. 191478-99-6, name is Methyl 4-amino-2,6-difluorobenzoate, A new synthetic method of this compound is introduced below., SDS of cas: 191478-99-6

4-(Chlorosulfonyl)benzoic acid (25.0 g, 113 mmol) and methyl 4-amino-2,6-difluorobenzoate (19.0 g, 101 mmol) were dissolved in methylene chloride (500 ml), and pyridine (25.0 ml, 285 mmol) was added thereto, followed by stirring at room temperature for 12 hours. The reaction solution was concentrated under reduced pressure. The obtained residue was diluted with water, and then the pH was adjusted to 1.0 by adding 6 N hydrochloric acid. The precipitated solid was filtered, and washed with water. The obtained solid was resuspended in water, and washed with a saturated aqueous sodium hydrogen carbonate solution, followed by extraction with ethyl acetate (100 ml×2). The pH of the obtained aqueous layer was adjusted to 6.0 by adding 6 N hydrochloric acid thereto, followed by extraction with ethyl acetate (100 ml×2). The extraction liquids were combined, washed with saturated aqueous sodium chloride, and dried over anhydrous sodium sulfate. Then, the solvent was removed to obtain the title compound (15.0 g, 36%). [0213] 1H NMR (d-DMSO, 400 MHz): delta 11.50 (s, 1H), 8.14 (d, J=8.4 Hz, 2H), 8.01 (d, J=8.4 Hz, 2H), 6.67 (d, J=10.4 Hz, 2H), 3.87 (s, 3H); MS (ESI) m/z 372 (M+H)+

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; AJINOMOTO CO., LTD.; Ueno, Hirokazu; Yamamoto, Takashi; Takashita, Ryuta; Yokoyama, Ryohei; Sugiura, Toshihiko; Kageyama, Shunsuke; Ando, Ayatoshi; Eda, Hiroyuki; Eviryanti, Agung; Miyazawa, Tomoko; Kirihara, Aya; Tanabe, Itsuya; Nakamura, Tarou; Noguchi, Misato; Shuto, Manami; Sugiki, Masayuki; Dohi, Mizuki; US2015/51395; (2015); A1;,
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These common heterocyclic compound, 57625-74-8, name is Methyl 2-methyl-2-phenylpropanoate, 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. Recommanded Product: Methyl 2-methyl-2-phenylpropanoate

(b) Reaction of Methyl-alpha,alpha-dimethylphenyl acetic acid with 4-Chlorobutyryl chlorideMethyl-alpha,alpha-dimethylphenylacetic acid on Fridel-Craft’s acylation with 4-chlorobutyryl chloride in presence of anhydrous aluminum chloride in ethylene dichloride produced acylated Methyl-alpha,alpha-dimethylphenyl acetic acid, i.e., ketone intermediate as meta and para- isomers.More particularly, aluminum chloride was taken in dichloroethane and cooled in between about 0 to 2O0C. To the above pre cooled solution, Methyl-alpha,alpha-dimethylphenyl acetic acid was added at low temperature. To the reaction mixture, 4-chlorobutyryl chloride was added between about 0 to 20C. After addition of acid chloride the reaction mixture was stirred for about 8 to 10 hours at the same temperature. After completion of the reaction, mixture was quenched over chilled mixture of potable water and cone, hydrochloric acid followed by stirring the reaction mixture for another 4 hours. The reaction mixture was washed with aqueous solution of sodium bicarbonate and finally with water. Removal of dichloromethane provided Methyl-4-(4-chloro-l-oxobutyryl)-alpha,alpha-dimethylphenyl acetate (Ketone) in about 95 % HPLC purity.EXAMPLE 2Methyl-4-(4-chloro-l-oxobutyryl)- a, a-dimethyl phenyl acetate (Ketone)95 Kg (0.7124 Kmole) of aluminium chloride was taken in 120 Ltr dichloroethane and reaction mixture was cooled to 0 to 2O0C. To it was added ester of example 1, 46 Kg (0.2584 Kmole) through addition flask, maintaining the temperature 0 to 200C. Finally, to the reaction mixture was added 80 Kg (0.5673 Kmoles) of 4-chlorobutyryl chloride through addition flask maintaining the temperature 0 to 200C. After addition of acid chloride stirred the reaction mixture at 0 to 200C for 8 to 10 hours. After completion it was quenched over chilled mixture of potable water and concentrated hydrochloric acid. Then stirred the reaction mixture at 0 to 200C for 4 hours and finally extracted in dichloroethane. It was washed with 10% w/v aqueous solution of sodium bicarbonate and finally with water. Removal of the solvent under vacuum provides thick oily mass of Methyl-4-(4-chloro-l-oxobutyryl)-alpha-alpha-dimethyl phenyl acetate (Ketone). HPLC purity = 95%. Yield = 65 to 70 Kg.

The synthetic route of Methyl 2-methyl-2-phenylpropanoate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; WOCKHARDT LIMITED; JAWEED MUKARRAM, Siddiqui, Mohammed; MERWADE, Aravind, Yekanathsa; KHAN, Anjum, Reyaz; SOLANKI, Pawan, Vrajlal; WO2007/7347; (2007); A1;,
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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. 2396-83-0, name is Ethyl hex-3-enoate, A new synthetic method of this compound is introduced below., Safety of Ethyl hex-3-enoate

A solution of 2.32 mL (14.5 mmol) ethyl (E)-hex-3-enoate in 30 mL dry dichloromethane under nitrogen was cooled to -78 C and 23.0 mL (23.0 mmol) DIBAL (1 m in dichloromethane) was added over 45 min. After stirring for 1 h methanol (8 mL) was added carefully, followed 50 mL of an aqueous citric acid solution (10 %, m/V). After warming up to room temperature 20 mL brine was added and the organic layer separated. The aqueous layer was extracted with dichloromethane (3 x 30 mL) and the combined organic layers dried over sodium sulfate and evaporated carefully (600 mbar, bath temperature 40 C). The liquid residue was treated with 1.14 g (16.4 mmol) hydroxylamine hydrochloride and 6.0 mL (6.0 mmol) sodium hydroxide solution (6 m) under ice cooling. The mixture was stirred for 4 h at room temperature, then 2 mL glacial acetic acid and 100 mL water added, followed by extraction with ethyl acetate (3 x 30 mL). The combined organic layers were dried over sodium sulfate and evaporated. The residue was purified by FSC (dichloromethane) to give 0.865 g (7.64 mmol, 53%) of the oxime 3 as a 1:1 E/Z mixture as an unstable pale yellow oil.

The synthetic route of 2396-83-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Lohrer, Bernhard; Bracher, Franz; Tetrahedron Letters; vol. 60; 51; (2019);,
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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. 87661-20-9, name is tert-Butyl cyclopropanecarboxylate, This compound has unique chemical properties. The synthetic route is as follows., Formula: C8H14O2

To a cooled solution (-40 C) of DIPEA (4.1 mL, 29.57 mmol, 2.1 eq) in THF (25 mL), was added w-BuLi (2.5M in hexanes, 1 1.2 mL, 28.36 mmol, 2 eq.) drop wise and the mixture was then stirred for 0.5 hr and then cooled to -78 C. Next, a solution of tert-butyl cyclopropanecarboxylate (2 g, 14.08 mmol, 1 eq.) in THF (5 mL) was added and the reaction mixture was stirred for 4 h at -78 C. 1-Propene, 3-bromo- (3.6 mL 42.25 mmol, 3 eq.) was added and reaction mixture was stirred for 2 h at -78 C. The reaction was then quenched with NH4Cl (30 mL) and extracted with DCM. The organic layer was dried over Na2S04 and concentrated to give tert-butyl 1-allylcyclopropane-l -carboxylate (1.5 g, 58 %). 1H NMR: (400 MHz, CDCl3) delta: 5.92-5.81 (m, 1H), 5.07-5.00 (m, 2H), 2.28 (d, J = 6.8 Hz, 2H), 1.45 (s, 9H), 1.15 (dd, J = 4.0, 3.2 Hz, 2H), 0.67 (dd, 4.0, 2.8 Hz, 2H).

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 87661-20-9.

Reference:
Patent; CAVION, INC.; RICHARDSON, Thomas E.; HIGGIN, Michelle; MACDONALD, Timothy; (102 pag.)WO2018/152317; (2018); A1;,
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Reference of 2967-93-3, 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. 2967-93-3 name is Methyl 2-fluoro-5-methylbenzoate, 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.

(Table B1, B36, Scheme B2-B3) N-(3,4-dichlorobenzyl)-5-(((4,5-dihydro-1H-imidazol-2-yl)amino)methyl)-2-fluorobenzamide Bromination step: A solution of methyl 2-fluoro-5-methylbenzoate (2.10 g, 12.49 mmol) (CAS No.2967-93-3 Combi Blocks) in CCl4 (60 mL) was allowed to reflux through a Dean Stark trap to remove trace amounts of water. The solution was cooled to ambient temperature and treated with N-bromosuccinimide (NBS) (2.44 g, 13.74 mmol) and 2,2’azobis(2-methylpropionitrile (AIBN) (0.20 g, 1.20 mmol). The solution was heated to reflux for an 18 hour period. The mixture was cooled to ambient temperature, filtered and the resulting filtrate was concentrated under reduced pressure. The crude was then purified on silica gel using EtOAc/hexanes as mobile phase. The desired fractions where concentrated under reduced pressure to afford methyl 5-(bromomethyl)-2-fluorobenzoate compound 1.9 g (61%): 1H NMR (400 MHz, CDCl3) delta 8.0 (m, 1H), 7.6 (m, 1H), 7.1 (m, 1H), 4.5 (s, 2H), 4.0 (s, 3H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl 2-fluoro-5-methylbenzoate, and friends who are interested can also refer to it.

Reference:
Patent; Vanderbilt University; Gogliotti, Rocco D.; Stauffer, Shaun R.; Jeon, KyuOk; Salovich, James M.; Macdonald, Jonathan D.; Mills, Jonathan J.; Meyers, Kenneth M.; Alvarado, Joseph R.; Han, Changho; Fesik, Stephen W.; Lee, Taekyu; (177 pag.)US2020/55824; (2020); A1;,
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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. 2459-25-8, name is Methyl 2-naphthoate, A new synthetic method of this compound is introduced below., Safety of Methyl 2-naphthoate

General procedure: The appropriate aryl-ester 18a-e (1 eq), was added of EtOH (2.22 ml*mmol/eq) followed by hydrazine monohydrate (3 eq). The solution was refluxed overnight, then cooled to room temperature. The precipitate obtained was filtered and washed with cold EtOH and n-hexane to give the pure product.

The synthetic route of 2459-25-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Giancotti, Gilda; Cancellieri, Michela; Balboni, Andrea; Giustiniano, Mariateresa; Novellino, Ettore; Delang, Leen; Neyts, Johan; Leyssen, Pieter; Brancale, Andrea; Bassetto, Marcella; European Journal of Medicinal Chemistry; vol. 149; (2018); p. 56 – 68;,
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Reference of 23676-08-6, These common heterocyclic compound, 23676-08-6, name is Methyl 4-ethoxybenzoate, 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.

General procedure: 4-dodecyloxy methylbenzoate(13.3 g, 0.04mol)was placed in a one liter single-necked round-bottom flask equippedwith double wall water condenser. Ethanol (250 ml) and potassium hydroxide (6 g, 0.1 mol)dissolved in distilled water (250 ml) were added to the flask. The solution was refluxed for2 hours and allowed to cool down at r.t. and then neutralized with 10% hydrochloric acidto get a white precipitate. It was purified by recrystallizing from methanol.

Statistics shows that Methyl 4-ethoxybenzoate is playing an increasingly important role. we look forward to future research findings about 23676-08-6.

Reference:
Article; Reddy, M. Kesava; Reddy, K. Subramanyam; Prakash; Narasimhaswamy; Molecular Crystals and Liquid Crystals; vol. 582; 1; (2013); p. 1 – 14;,
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Synthetic Route of 945-93-7, A common heterocyclic compound, 945-93-7, name is Ethyl 3-phenylbut-2-enoate, molecular formula is C12H14O2, 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.

General procedure: Unsaturated ester (4a-4d) (0.1 mol) was boiled with 5 N NaOH under a reflux condenser for 2-3 h and left to stir at room temperature overnight. The formed carboxylate salt was dissolved in water and diluted HCl was added. The obtained solid product was filtered and crystallized with EtOH-water. (E) -3-Phenylbut-2-enoic acid (3d) [34]: Yield: 15 g, 94%. Mp: 90-92 C, (lit: 90-92 C). 1 H NMR (400 MHz, CDCl3) , delta (ppm): 7.51-7.49 (3H, m), 7.40-7.38 (2H, m), 6.18 (1H, s), 2.61 (3H, s).

The synthetic route of 945-93-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Sari, Sait; Uenalan, Seda; Yilmaz, Mehmet; Turkish Journal of Chemistry; vol. 43; 6; (2019); p. 1656 – 1671;,
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Application of 18595-13-6, 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. 18595-13-6, name is Methyl 2-amino-6-methylbenzoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Step 2. Preparation of 2-Isopropoxycarbonylamino-6-methyl-benzoic acid methyl ester. Add isopropyl chloroformate (19.8 mL, 19.8 mmol, 1.0 M in toluene) dropwise to a solution of 2-Amino-6-methyl-benzoic acid methyl ester (3.27 g, 19.8 mmol) and pyridine (4.0 mL, 50 mmol) in dichloromethane (39 mL) at 0C under an atmosphere of nitrogen and stir at room temperature for 14 h. Add 1M HCl and separate the layers. Extract the aqueous layer with dichloromethane. Dry the organic layer over anhydrous sodium sulfate, filter, and remove the solvent under reduced pressure. Purify the residue by flash chromatography, eluting with hexanes/ethyl acetate, to afford the title compound (3.80 g, 76%) :’H NMR (CDCl3) 8 1.29 (d, J = 6.5 Hz, 6H), 2.43 (s, 3H), 3.94 (s, 3H), 5.00 (septuplet, J = 6.5 Hz, 1H), 6.90 (d, J = 8.1 Hz, 1H), 7.32 (t, J = 8.1 Hz, 1H), 8.07 (d, J = 8.1 Hz, 1H), 8.86 (brs, 1H). MS (ES+): 252 (M+H).

The synthetic route of Methyl 2-amino-6-methylbenzoate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ELI LILLY AND COMPANY; WO2005/37796; (2005); A1;,
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