Category: 609-12-1

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. 609-12-1, name is Ethyl 2-bromo-3-methylbutanoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of Ethyl 2-bromo-3-methylbutanoate

A solution of pyrazine-2-carbothioamide (1 g, 7.19 mmol) in ethanol (10 ml) was treated with ethyl 2-bromoisovalerate (2.25 g, 10.8 mmol), and pyridine (853 mg, 872 mul, 10.8 mmol) is combined to give a dark brown suspension. and heated to 100 C. for 6 hours in a sealed tube. The reaction mixture was cooled and concentrated to dryness under reduced pressure, and the resulting suspension is extracted with ethyl acetate (3*50 mL). The organic layers were combined, washed with saturated NaHCO3 (1*50 mL), saturated sodium chloride (2*20 mL). The organic layers were dried over MgSO4 and concentrated in vacuo to give 5-isopropyl-2-pyrazin-2-yl-thiazol-4-ol (260 mgs, 16%) which was used directly without further purification.

The synthetic route of 609-12-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Alam, Muzaffar; Du Bois, Daisy Joe; Hawley, Ronald Charles; Kennedy-Smith, Joshua; Minatti, Ana Elena; Palmer, Wylie Solang; Silva, Tania; Wilhelm, Robert Stephen; US2011/71150; (2011); A1;,
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Application of 609-12-1, 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. 609-12-1, name is Ethyl 2-bromo-3-methylbutanoate, This compound has unique chemical properties. The synthetic route is as follows.

[00485] 2-(1’Benzyl’2-methyl-1H-indol-4’yloxy)-3-methyl-butyric acid ethyl ester 7:1-Benzyl-2-methyl-1H-indol-4-ol 3 (0.3 g 1.26 mmole) was dissolved in anhydrous dimethylformamide (20 ml_). To the solution sodium hydride 60% in mineral oil (66 mg 1.65 mmole) was added. The mixture was stirred at room temperature for 1 h. To the mixture ethyl-2-bromoisovalerate (0.344 mL, 1.65 mmole) was added. The mixture was stirred at room temperature for 18 h. The reaction was diluted with ethyl acetate (300 mL) and washed with H2O (4 x 100 mL) and brine (1 x 100 mL). The organic layer was separated, dried with magnesium sulfate and concentrated. The residue was purified by column chromatography (10:1 Hexane:EtOAc) to afford a 1 :1 mixture of 7:ethyl-2-bromoisovalerate. Further purification by column chromatography (10:1 Hexane.epsilontOAc) afforded 7 (0.09 g, 19 %) as a yellow oil.

The chemical industry reduces the impact on the environment during synthesis Ethyl 2-bromo-3-methylbutanoate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; ILYPSA, INC.; WO2007/56279; (2007); A2;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Reference of 609-12-1,Some common heterocyclic compound, 609-12-1, name is Ethyl 2-bromo-3-methylbutanoate, molecular formula is C7H13BrO2, 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.

52.4 g of activated zinc powder and 450 ml of anhydrous THF,Add a few drops under N2 protectionEthyl alpha-bromoisovalerate2 to trigger the reaction,66 reflux 45min stirring until the reaction liquid becomes dark green after adding 20.324g (0.165mol)Cyclohexyl acetonitrile,And slowly add 2 (88.71 g, 0.4243 mol) within 1 h,Continue to reflow 1H stop heating, cooled to room temperature,Add 80ml 50% K2CO3 solution was stirred vigorously for 10min, the reaction solution was allowed to stratification, the organic phase was separated, the residue was extracted with THF,The combined organic phases were hydrolyzed by adding 150 ml of 15% HCl, the organic layer was separated and concentrated under reduced pressure, the aqueous layer was extracted three times with ethyl acetate,The combined organic phases were washed three times with saturated sodium bicarbonate solution, saturated NaCl, dried over anhydrous Na2SO4,The solvent was removed under reduced pressure to give compound 3 as a crude reddish brown liquid, 38.4 g, which was used directly in the next reaction without purification.

The synthetic route of 609-12-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Yunnan University; Chinese Academy Of Sciences Kunming Animal Institute; He Yanping; Zheng Yongtang; Zhang Yufang; Xiang Siying; Zhang Hongbin; Zhao Zhidong; Yang Liumeng; (9 pag.)CN106866548; (2017); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Application of 609-12-1, A common heterocyclic compound, 609-12-1, name is Ethyl 2-bromo-3-methylbutanoate, molecular formula is C7H13BrO2, 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.

A solution of 2-bromo-3-methyllpropanoic acid ethyl ester (0.418 g, 2 mmol) and 4-bromobenzylthiol (0.402 g, 2 mmol) in DMF (5 mL) was cooled to 0 C and treated with K2CO3 (0. 414 G, 3. mmol). After stirring for 2 h, the reaction was quenched with 5% HC1 (15 mL) and diluted with ethyl acetate (50 mL). After seperation, the aqueous layer extracted with ethyl acetate (3 x 15 mL). The combined organic layers were washed with sat. aq NACL, dried over MGS04 and concentrated. Purification by flash column chromatography (5% ethyl acetate in heptane) provided (4-bromophen-yl-4-methylsulfanyl)-3- methylbutanoic acid ethyl ester (660 MG, 90%) as white solid. 1H NMR (CDC13), 7.43 (d, J = 8 Hz, 2 H), 7.18 (d, J = 8 Hz, 2 H), 4.17 (q, J = 6 Hz, 2 H), 3.75 (s, 2 H), 2.85 (d, J = 9 Hz, 1 H), 2.04 (m, 1 H), 1.29 (t, J = 6 Hz, 3 H), 1.02 (d, J = 6 Hz, 3 H), 0.98 (d. J = 6 Hz, 3 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; THE INSTITUTE OF PHARMACEUTICAL DISCOVERY, LLC; WO2004/99170; (2004); A2;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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. 609-12-1, name is Ethyl 2-bromo-3-methylbutanoate, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C7H13BrO2

Under a nitrogen atmosphere, 4. 07 g of potassium ethoxide and 150 mL of purified tetrahydrofuran were added to a 250 mL three-necked flask equipped with a refluxing device and 8 g of ethyl 2-cyclopentyl-2-cyanoacetate was added. The reaction was stirred at room temperature (about 25 C). And then slowly added dropwise to a solution of ethyl 2-bromoisovalerate (9. 2 g) in 50 mL of tetrahydrofuran,And the mixture was heated under reflux for 8 hours. The solvent was then removed by evaporation to give a red viscous liquid and a mixture of white solids. Extracted with ether, washed with water, 5% sodium hydrogencarbonate, and then washed with water until the organic phase was neutral. The organic phase was dried over anhydrous magnesium sulphate for 12 h. Filtering, concentrating the solvent to obtain crude product, and then vacuum distillation, the unreacted raw materials and low boiling point of the material evaporated, 2-cyclopentyl-3-isopropyl-2-cyano-succinate 9. 5 g. The mass spectrum and infrared spectrum of the product were consistent with the structure of the target compound.

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 609-12-1.

Reference:
Patent; China Petroleum & Chemical Corporation; SINOPECBeijing Research InstituteofChemicalIndustry; XIE, LUNJIA; TIAN, YU; FENG, ZAIXING; ZHAO, SIYUAN; SUN, ZHUFANG; (18 pag.)CN104418770; (2016); B;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Electric Literature of 609-12-1, These common heterocyclic compound, 609-12-1, name is Ethyl 2-bromo-3-methylbutanoate, 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.

Under an atmosphere of nitrogen, an ice-cooled solution of 6-methoxyisoindolin-1-one (commercially available from for example Astatech) (105 mg, 0.64 mmol) in DMF (2.5 mL) was treated with sodium hydride (60% w/w in mineral oil) (31 mg, 0.77 mmol) and the mixture was allowed to warm to ambient temperature. The mixture was then treated with ethyl 2-bromo-3-methylbutanoate (commercially available from for example Alfa Aesar) (135 mg, 0.64 mmol) and the mixture was stirred for 18 hours then cautiously treated with saturated aqueous ammonium chloride (20 mL). The product was extracted with ethyl acetate (2*25 mL) and the combined organic phase was washed with water (20 mL), brine (20 mL), filtered through a hydrophobic fit and evaporated to dryness. the product was purified by flash chromatography (20 g silica cartridge) using a gradient elution from 0 to 50% ethyl acetate in cyclohexane to afford the title compound (40 mg, 21% yield). LCMS RT=1.03 min, ES+ve m/z 292 [M+H]+

The synthetic route of 609-12-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Crews, Craig M.; Buckley, Dennis; Ciulli, Alessio; Jorgensen, William; Gareiss, Peter C.; Van Molle, Inge; Gustafson, Jeffrey; Tae, Hyun-Seop; Michel, Julien; Hoyer, Dentin Wade; Roth, Anke G.; Harling, John David; Smith, Ian Edward David; Miah, Afjal Hussain; Campos, Sebastien Andre; Le, Joelle; US2014/356322; (2014); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

These common heterocyclic compound, 609-12-1, name is Ethyl 2-bromo-3-methylbutanoate, 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. COA of Formula: C7H13BrO2

General procedure: Benzenesulfonamide (1.2mmol), ethyl alpha-bromophenylacetate or ethyl pheny-lacetate (2.4mmol), and toluene (4mL)werecombinedinasealedtubeequippedwith astirbar.Themixturewasstirredat50Cfor10min,TiCl4 (1.8 mmol) was added, andthereactionmixturewasheatedto115C.Afteravariableperiodoftimethe mixturewasdilutedwithH2O (10mL)toremovetheexcessofTiCl4, filtered,andextracted withAcOEt(3×15mL). The combined organic layers were dried over anhydrous Na2SO4 and thesolventwasevaporatedinvacuo.Crudecompoundswere purified by flash column chromatography (silicagel;cyclohexane=AcOEt 8:2). 2-Bromo-3-methyl-N-[(4-methylphenyl)sulfonyl]butanamide (4b). Orange oil, 57% yield; IR(KBr) 3528, 3235, 2970, 2880, 1718, 1597, 1450, 1171, 1085, 865, 550 cm-1; 1H NMR (CDCl3) d0.94 (d, 3H, J 6.6 Hz, CH3), 0.96 (d, 3H, J 6.6 Hz, CH3), 2.21 (octuplet, 1H, CH3CHCH3), 2.44 (s,3H, CH3Ph), 4.08 (d, 1H, J 6.0 Hz, CHBr), 7.34 (d, 2H, J 8.1 Hz, CH Ar), 7.91 (d, 2H, J 8.1 Hz,CH Ar), 9.01 (broad s, 1H, NH); 13C NMR (CDCl3) d 20.0 and 20.3 (CH3), 21.7 (CH3Ph), 32.4(CH3CHCH3), 58.1 (CHBr), 128.5 and 129.6 (CH Ar), 134.7 (CS Ar), 145.5 (CCH3 Ar), 166.1(CONH); Anal calcd for C12H16BrNO3S: C 43.12; H 4.83; N 4.19; found C 42.99; H 4.81; N 4.18%.

The synthetic route of Ethyl 2-bromo-3-methylbutanoate has been constantly updated, and we look forward to future research findings.

Reference:
Article; Ammazzalorso, Alessandra; Tricca, Maria Luisa; Bruno, Isabella; De Filippis, Barbara; Di Matteo, Mauro; Fantacuzzi, Marialuigia; Giampietro, Letizia; Maccallini, Cristina; Mollica, Adriano; Amoroso, Rosa; Synthetic Communications; vol. 45; 22; (2015); p. 2546 – 2554;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Reference of 609-12-1,Some common heterocyclic compound, 609-12-1, name is Ethyl 2-bromo-3-methylbutanoate, molecular formula is C7H13BrO2, 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 11.12b: Compound (5-33) KOH, THFZH2Oily-V-33[00438] 3-Methyl-2-(2-methyl~1H-indol-4’yloxy)-butyric acid ethyl ester (2): A mixture of 4-hydroxy-2-methylindoie (1) (1.5 g, 0.010 mole), 2-bromo-3-methyl-butyric acid ethyl ester (2.2 g, 0.010 mole) and potassium carbonate (excess) in acetone (50 mL) was refluxed for 3 days. The reaction mixture was filtered, and the filtrate was concentrated. The residue was purified by column chromatography (20:1 Hex:EtOAc) to afford intermediate 2. Yield: 1.88 g, 71 %

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Ethyl 2-bromo-3-methylbutanoate, its application will become more common.

Reference:
Patent; ILYPSA, INC.; WO2007/56279; (2007); A2;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Some common heterocyclic compound, 609-12-1, name is Ethyl 2-bromo-3-methylbutanoate, molecular formula is C7H13BrO2, 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. name: Ethyl 2-bromo-3-methylbutanoate

4-fluoro-3-nitrophenol (500 mg, 3.18 mmol) was dissolved in DMF (6.365 mL) at room temperature. Cesium Carbonate (1244 mg, 3.82 mmol) was added followed by ethyl 2-bromo-3-methylbutanoate (0.574 mL, 3.50 mmol). The mixture was stirred at 60 C. Reaction left at 60 C overnight. Reaction was then diluted with water and a precipitate formed. The solid was filtered off and dried on high vacuum overnight to yield 83A (tan solid, 615 mg, 2.156 mmol, 67.7 % yield), yield). LC-MS Anal. Calc’d for Ci3Hi6FN05 285.10, Tr = 1.04 min (Method A) (Note: product does not ionize well). NMR (400 MHz, MeOH-d4) delta: 7.60 (dd, J=6.0, 3.3 Hz, 1H), 7.53 (dd, J=10.9, 9.3 Hz, 1H), 7.38 (s, 1H), 4.84 (d, J=4.8 Hz, 1H), 4.16 (dd, J=7.1, 2.8 Hz, 2H), 2.20-2.30 (m, 1H), 1.15-1.20 (m, 3H), 1.01 (dd, J=6.8, 4.6 Hz, 6H) 83B.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 609-12-1, its application will become more common.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; BALOG, James Aaron; CHERNEY, Emily Charlotte; MARKWALDER, Jay A.; SHAN, Weifang; WILLIAMS, David K.; (203 pag.)WO2016/210414; (2016); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Synthetic Route of 609-12-1,Some common heterocyclic compound, 609-12-1, name is Ethyl 2-bromo-3-methylbutanoate, molecular formula is C7H13BrO2, 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.

in room temperature,2-(2-Methyl-1,3-dioxolan-2-yl)ethan-1-amine (Compound 2) (28.86 g, 220 mmol) was first dissolved in acetonitrile.The above solution was then added to 3-bromo-4-ethoxy-4-methyl-4-oxobutan-1-yl hydrazone with stirring.(Compound 1) (41.61 g, 200 mmol) and triethylamine (42 mL, 302 mmol) EtOAc.The resulting mixture was stirred at room temperature overnight.Pour into 500 mL of ether.The resulting suspension was extracted with 300 mL of water.It was extracted twice with 300 mL of 2 mol/L hydrochloric acid.The combined extracts were basified by the addition of a 25% aqueous sodium hydroxide solution and extracted twice with 500 mL x 2 ethyl acetate.The extracts were combined and washed successively with water and saturated brine.It was dried over anhydrous magnesium sulfate. After removing the desiccant by filtration,Solvent volatilization,45.54 g of yellow (2-(2-methyl-1,3-dioxolan-2-yl)ethyl)proline ethyl ester were obtained(Compound 3),The yield was 87.8%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Ethyl 2-bromo-3-methylbutanoate, its application will become more common.

Reference:
Patent; Li Huaxu; (9 pag.)CN108164517; (2018); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics