Month: June 2021

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. 541-16-2, name is Di-tert-Butyl malonate, A new synthetic method of this compound is introduced below., Recommanded Product: Di-tert-Butyl malonate

A solution of sodium hydride (0.040 g, 1.54 mmol) in THF (100mL) was cooled to 0C and treated with di-tert-butyl malonate (20.7 3 mL, 92.47 mmol) dropwise via dropping funnel, over 20 min. After stirring at room temperature for 30 min., 3,3-dimethylallyl bromide (9.7 mL, 83.22 mmol) was added. After stirring an additional 19 h, the reaction mixture was diluted with 10% HCl solution (100 mL) and EtOAc (100 mL). The resulting organic phase was washed with satd. aq. NaCl, dried over MgSO4, filtered, and concentrated to afford 25.74 g (94%)of a crude yellow oil. TLC: Rf 0.60 (silica, 10% ethyl acetate-hexane).

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 Corporation; EP923530; (2004); B1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 64113-91-3, name is tert-Butyl 2-aminobenzoate, 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 64113-91-3, Recommanded Product: tert-Butyl 2-aminobenzoate

To a solution of [4- (PHENYLMETHYL) PHENYL] acetic acid (0.059g, 0. 26MMOL, 1 EQUIV) and DIPEA (0. 054ML, 0. 31MMOL, 1.2equiv) in anhydrous DMF (0. 5MOI) was added a solution of HATU (0.119g, 0. 31MMOL, 1.2equiv) in DMF (0. 5M1), FOLLOWED by 1,1- dimethylethyl 2-aminobenzoate (0.060 g, 0. 31mmol, 1.2equiv) in DMF (0. 5ml). The mixture was stirred under an atmosphere of nitrogen for 72 hr, then concentrated under reduced pressure and partitioned between DCM and 2N HCI. The separated organic phase was washed with saturated sodium bicarbonate then evaporated under a stream of nitrogen and purified by preparative h. p. l. c. to give the title compound (0.033g, 32%) as a white solid ; LC/MS : m/z 402.2 [MH] +.

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

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2005/16870; (2005); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

57486-67-6, name is Methyl 2-(2-fluorophenyl)acetate, belongs to esters-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Quality Control of Methyl 2-(2-fluorophenyl)acetate

EXAMPLE 4 4-[(R,S)-2-(2-Fluorophenyl),propyl]-1-{(R,S)-2-fluoro-3-[5-(1,2,4-triazol-4-yl)-1H-indol-3-yl]propyl}pipeperazine Methyl 2-fluorophenylacetate (24.2 g, 0.144 mol) in THF (75 ml) was added dropwise over 20 min to a -78 C. solution of LDA (diisopropylamine (16.0 g, 0.158 mol) and n-butyl lithium (2.5 M, 61 ml)) in THF (300 ml) and stirring was continued for 1 h. Methyl iodide (22.5 g, 0.158 mol) was added dropwise over 15 min and the reaction mixture allowed to warm to room temperature over 1 h. The solution was poured into saturated ammonium chloride solution and extracted with diethyl ether. The extract was washed with brine, dried and evaporated to yield methyl 2-(2-fluorophenyl)propanoate (26.2 g, 100%) as an oil.

The synthetic route of 57486-67-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Merck Sharp & Dohme Ltd.; US5977116; (1999); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Related Products of 52727-57-8, 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. 52727-57-8, name is Methyl 2-amino-5-bromobenzoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Compound 1a (18.60 g, 80.85 mmol) was dissolved in concentrated hydrochloric acid (200 mL, 12N), and an aqueous solution of sodium nitrite (6.69 g, 97.02 mmol) was slowly added dropwise at -10 to 0C. The reaction solution was at 0C. Stir for 1 hour. This reaction was added dropwise to a mixture of cuprous chloride (800 mg, 8.09 mmol) and sulfur dioxide (15.54 g, 242.55 mmol) at 0C. The resulting reaction solution was stirred at 0 C. for 1 hour and further warmed to 20 C. and stirred for 3 hours. After the reaction was completed, it was extracted with ethyl acetate (200 mL×3). The organic phases were combined, dried, concentrated to dryness under reduced pressure, and separated and purified by column chromatography on silica gel (petroleum ether/ethyl acetate=100-0%) to give Compound 1b (4.10 g).

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-amino-5-bromobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Zhengda Tianqing Pharmaceutical Group Co., Ltd.; Nanjing Mingde Drug Discovery Co., Ltd.; Yao Yuanshan; Chen Bin; Chen Yuan; Li Ao; Xu Ran; Huang Zhensheng; Tian Dongdong; Li Hongwei; Yang Chengshuai; Li Jian; Chen Shuhui; (26 pag.)CN107987072; (2018); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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. 394-35-4, name is Methyl 2-fluorobenzoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C8H7FO2

A mixture of 20.0 g of methyl 2-fluorobenzoate, 15.2 g of methyl thioglycolate, 21.8 g of potassium carbonate,and 150 ml of N,N-dimethylformamide was stirred for 4 hours at 60°C. After the reaction mixture was cooled to roomtemperature, water was added thereto, and the residue was washed three times with tert-butyl methyl ether. Concentratedhydrochloric acid was added to the aqueous layer, and then extraction was performed three times by using tert-butylmethyl ether. The collected organic layer was washed with water and saturated saline, dried over magnesium sulfate,and then concentrated under reduced pressure. The residues were recrystallized from ethanol and water, therebyobtaining 3.89 g of methyl 3-hydroxybenzo[b]thiophene-2-carboxylate.

The synthetic route of 394-35-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sumitomo Chemical Company Limited; MUKUMOTO, Fujio; TAMAKI, Hiroaki; KUSAKA, Shintaro; IWAKOSHI, Mitsuhiko; EP2926660; (2015); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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. 478375-40-5, name is Methyl 3-bromo-5-methylbenzoate, A new synthetic method of this compound is introduced below., Computed Properties of C9H9BrO2

AIBN (2,2′-azobis(2-methylpropionitrile)) (1.79 g) was added to methyl 3-bromo-5- methylbenzoate (50 g) and N-bromosuccinimide (44.7 g) in 350 mL acetonitrile, and the mixture was refluxed overnight. An additional 11 g of N-bromosuccinimide and 0.5 g of AIBN (2,2′-azobis(2- methylpropionitrile)) was added, and the re fluxing was continued for 3 hours. The mixture was concentrated, and then taken up in 500 mL ether, and stirred for 30 minutes. The mixture was then filtered, and the resulting solution was concentrated. The crude product was chromatographed on silica gel using 10% ethyl acetate in heptane to give 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; ABBVIE INC.; BENATUIL, Lorenzo; BRUNCKO, Milan; JUDD, Andrew, S.; LI, Yingchun; MCCLUSKEY, Andrew; PHILLIPS, Andrew, C.; PHILLIPS, Darren, C.; SEAGAL, Jane; SOUERS, Andrew, J.; (608 pag.)WO2017/214458; (2017); A2;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Synthetic Route of 394-35-4, 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. 394-35-4 name is Methyl 2-fluorobenzoate, 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.

General procedure: Compounds 6a-t were synthesized from substituted benzoic acid via six steps according to the literature method as described. Various substituted benzoic acids 1a-t were treated with SOCl2 to give compounds 2a-t, which were reacted with CH3OH and EtN3 in CH2Cl2 at 0 to afford compounds 3a-t. Compounds 4a-t were prepared by the reaction of compounds 3a-t, hydrazine hydrate in CH3OH under reflux condition about 5h. Subsequently, compounds 5a-t were obtained by reaction of compounds 4a-t with CS2 and KOH in CH3OH. Compounds 6a-t were obtained by the cyclization reaction of compounds 5a-t in the presence of HCl at 0-5°C.

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

Reference:
Article; Li, Liangjing; Ding, Hao; Wang, Baogang; Yu, Shichong; Zou, Yan; Chai, Xiaoyun; Wu, Qiuye; Bioorganic and Medicinal Chemistry Letters; vol. 24; 1; (2014); p. 192 – 194;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 15964-79-1, name is Methyl 2-(3,4-dimethoxyphenyl)acetate, 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 15964-79-1, HPLC of Formula: C11H14O4

Manufacturing Example 13: Preparation of 2-(3,4-Dimethoxyphenyl) acetaldehyde (52) Anhydrous diethyl ether solution containing methyl 3′,4′-dimethoxyphenyl acetate (1.94 g, 9.24 mmol) was stirred, during which DIBAL-H (11.1 mL, 1 M in THF solution) was added thereto drop by drop with maintaining the temperature at -78C. The mixture was stirred at the same temperature for 1 hour. Rochelle aqueous solution was carefully added thereto for 15 minutes. The mixture of the two phases was stirred vigorously at 0 C for 1 hour, which was added to water. The water layer was extracted with EtOAc (*2) and the organic layer was dried over MgSO4, filtered and concentrated under reduced pressure. Then, the obtained residue was purified by flash column chromatography (EtOAc:n-hexane=1:2) to give the compound 52 of Manufacturing Example 13 (yield: 68%, 1.13 g). 1H NMR (CDCl3, 300 MHz) delta 9.66 (t, 1H, J = 2.5 Hz), 6.80 (d, 1H, J = 8.0 Hz), 6.68 (m, 1H), 6.64 (d,

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl 2-(3,4-dimethoxyphenyl)acetate, and friends who are interested can also refer to it.

Reference:
Patent; SNU R&DB Foundation; SUH, Young-Ger; CHANG, Dong-Jo; AN, Hongchan; KIM, Kyu-Won; KIM, Young-Myeong; LEE, Ho-Young; EP2871187; (2015); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Synthetic Route of 1731-79-9, These common heterocyclic compound, 1731-79-9, name is Dimethyl dodecanedioate, 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 cooled (0 C) solution of LiAlH4 (1.73 g, 45.6 mmol) in THF (280 mL) was added a solution ofdimethyl dodecanedioate (4.35 g, 15.2 mmol) in THF (20 mL) dropwise, and the resulting solution wasstirred at 0 C for 3 h. Then, the reaction mixture was quenched with MeOH and 1 M HCl. The organic layer wasseparated and the aqueous layer was extracted with diethyl ether three times. The combined organic layer was washedwith water and brine, and dried over sodium sulfate. After evaporation of the solvent, the product was obtained(3.22 g, 92%) in high purity, which was then used in the next step without further purification.1H-NMR (500 MHz, CDCl3): delta3.64 (t, J =7.5 Hz, 4H, 1-H, 14-H), 1.57 (m, 4H, 2-H, 13-H), 1.35-1.26(20H, 3-H to 12-H)13C-NMR (125 MHz, CDCl3): delta63.1 (C1, C14), 32.8 (C2, C13), 29.6, 29.6, 29.5, 29.4 (C4 to C11), 25.7(C3, C12)HR-MS (ESI-TOF): m/z calcd for C14H30O2Na [M+Na]+ 253.2138, found 253.2137IR (film): 3409, 3347, 2923, 2854 cm

The synthetic route of 1731-79-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Tonoi, Takayuki; Kawahara, Ryo; Yoshinaga, Yutaka; Inohana, Takehiko; Fujimori, Keiko; Shiina, Isamu; Tetrahedron Letters; vol. 56; 11; (2015); p. 1356 – 1359;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Related Products of 23426-63-3,Some common heterocyclic compound, 23426-63-3, name is Methyl 2-bromo-2-methylpropanoate, molecular formula is C5H9BrO2, 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.

Step B; 2,5-Dimethyl-4-thiocyanato-phenol 82 (5.75 g, 32.1 mmol) is dissolved in acetonitrile (25 mL) . Powdered cesium carbonate (15.32 g, 47.0 mmol) is added. Then 2-bromo-2- methyl-propionic acid methyl ester (4.50 mL, 34.8 mmol) is added and the mixture is stirred at 600C for 18 h. Filtration and concentration, followed by silica gel chromatography (0- 50% ethyl acetate in hexanes) yielded 2- (2, 5-dimethyl-4- thiocyanato-phenoxy) -2-methyl-propionic acid methyl ester 83 as an oil: 1H-NMR (400 MHz, CDCl3) (rotamers are present; the data given is for the most abundant isomer) delta = 7.39 (s, IH), 6.50 (S, IH), 3.78 (s, 3H)7 2.42 (s, 3H), 2.20 (s, 3H), 1.62 (s, 6H). MS calcd. for C14H17NNaO3S (M+Na+) 302.1, found 302.1.

The synthetic route of 23426-63-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; IRM LLC; WO2007/56366; (2007); A2;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics