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. 56525-63-4, name is Methyl 3-chloro-4-methylbenzoate, A new synthetic method of this compound is introduced below., name: Methyl 3-chloro-4-methylbenzoate

To a solution of methyl 3-chloro-4-methylbenzoate (5.0g, 27.1mmol) in carbon tetrachloride (50ml) were added NBS (5.8g, 32.0mmol) and AIBN (0.442g, 2.70mmol). The mixture was stirred at reflux for 18h. The mixture was al­lowed to cool to room temperature and then concentrated in vacuo. The residue was purified by flash chromatography on silica (eluant EtOAc:pet. ether 0:100 to 5:95); yield 5.96g (84%).

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; FERRING B.V.; WO2006/18443; (2006); A1;,
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Some common heterocyclic compound, 150529-73-0, name is Methyl 2-(3-bromophenyl)acetate, molecular formula is C9H9BrO2, 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: Methyl 2-(3-bromophenyl)acetate

INTERMEDIATE 72-(3-BromophenyD-2-methylpropionic acid methyl esterA solution of Intermediate 6 (15.85 g, 69.2 mmol) in THF (50 mL) was added as a steady stream over about 5 minutes to a suspension of sodium hydride (60% dispersion in mineral oil, 8.32 g, 208 mmol) in THF (100 mL) under nitrogen in an ice-water bath whilst maintaining the internal temperature between 1O0C and 200C. After the addition was complete, the mixture was stirred at r.t. for 1 h. The mixture was cooled again in an ice-water bath, and a solution of methyl iodide (10.6 mL, 24.6 g, 173 mmol) in THF (100 mL) was added slowly so as to maintain the temperature of the reaction at <25C. After the addition was complete the mixture was stirred for a further 15 minutes with the ice- water bath, and then for 18 h. The mixture was poured slowly (over a period of about 2 minutes) onto a mixture of ice (approximately 100 g) and saturated ammonium chloride solution (100 mL). The resulting mixture was evaporated and extracted with DCM (2 x 50 mL). The combined organic phases were dried (MgSO4), the solvent removed in vacuo and purified by column chromatography (SiO2, 10-100% EtOAc in heptane) to give the title compound (17.3 g) as a pale straw-coloured oil. deltaH (CDCl3) 7.48 (t, IH), 7.38 (m, IH), 7.23-7.29 (m, IH), 7.19 (t, IH), 3.66 (s, 3H), 1.56 (s, 6H). These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 150529-73-0, its application will become more common. Reference:
Patent; UCB PHARMA S.A.; BUeRLI, Roland; HAUGHAN, Alan, Findlay; MACK, Stephen, Robert; PERRY, Benjamin, Garfield; RAPHY, Gilles; SAVILLE-STONES, Elizabeth, Anne; WO2010/52448; (2010); A2;,
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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. 111-61-5, name is Ethyl stearate, A new synthetic method of this compound is introduced below., Formula: C20H40O2

General procedure: To a solution of 100 mg of compound 3 (55 mumol, 1 equiv) in 2 ml of corresponding fatty ester (excess), 100 mg of Lipozyme was added. The reaction was set under rotary evaporator at 50 C during 8 to 14 hours depending on the corresponding fatty ester. Lipozyme was filtered, and the solution was purified directly on silica gel (from pure EtOAc to EtOAc/MeOH 4:1(v/v)), giving white solid. Yields: 4 (80mg): 74%, 5 (75mg): 68%, 6 (72mg): 64%, 7 (69mg): 60%.

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:
Article; Miao, Yong; Djedani-Pilard, Florence; Bonnet, Vronique; Beilstein Journal of Organic Chemistry; vol. 10; (2014); p. 2654 – 2657;,
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Synthetic Route of 24812-90-6,Some common heterocyclic compound, 24812-90-6, name is Methyl 3-amino-4-methoxybenzoate, molecular formula is C9H11NO3, 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.

Anhydrous p-toluene sulfonic acid (25.0 g, 137.43 mmol) was melted at 120 C and 3-amino-4-methoxy benzoic acid methyl ester (10 g, 55.25 mmol) obtained in step 1 of Preparation Example 1 and 2,4-difluorobenzonitrile (11.53 g, 82. 87 mol) were added thereto and stirred at 160 C for 8 hours. The resulting solution was cooled to room temperature and the reaction was stopped by adding NaHCO3 thereto. The resulting mixture was extracted with ethyl acetate, the extract was dried over MgSO4 and concentrated under a reduced pressure. The resulting residue was purified by silica gel column chromatography to obtain the title compound (10.0 g, 31.22 mmol) in a yield of 57 %. 1H NMR (CDCl3): delta 8.31-8.22 (1H, m), 7.82-7.79 (1H, d), 7.65 (1H, s), 7.02-6.85 (3H, m), 3.88 (6H, s) MW: 320

The synthetic route of 24812-90-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CRYSTALGENOMICS, INC.; YUYU INC.; WO2004/65370; (2004); A1;,
Ester – Wikipedia,
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Synthetic Route of 63485-50-7, 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. 63485-50-7, name is cis-Methyl 3-hydroxycyclobutanecarboxylate, This compound has unique chemical properties. The synthetic route is as follows.

Triphenylphosphine-PS (3.27 g, 12.5 mmol) was added to a solution of 2- (difluoromethoxy)-5-fluorophenol (Intermediate 2D) (1 .85 g, 10.4 mmol) in tetrahydrofuran (10 mL). The reaction mixture was cooled to 0 C, and (c/s)-methyl 3- hydroxycyclobutanecarboxylate (1 .33 mL, 12.5 mmol) was added, followed by DIAD (2.4 mL, 13 mmol). The reaction mixture was then warmed to room temperature, stirred for 12 h, filtered, and concentrated. The remaining material was purified on silica gel eluting with a 0%-70% EtOAc-hexanes gradient. The appropriate fractions were combined, evaporated under reduced pressure and placed in vacuo to give the title compound (1 .79 g, 58%). 1H NMR (400 MHz, CD3SOCD3) delta 2.27-2.45 (m, 2 H), 2.57-2.79 (m, 2 H), 3.13-3.27 (m, 1 H), 3.32 (s, 3 H), 4.90 (dd, J = 7, 6 Hz, 1 H), 6.66-6.95 (m, 2 H), 7.03 (s, 1 H), 7.1 1 – 7.34 (m, 1 H); LC-MS (LC-ES) peak at T = 0.86 min.

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

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; DEATON, David Norman; GUO, Yu; HANCOCK, Ashley Paul; SCHULTE, Christie; SHEARER, Barry George; SMITH, Emilie Despagnet; STEWART, Eugene L.; THOMSON, Stephen Andrew; (556 pag.)WO2018/69863; (2018); 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. 1260092-46-3, name is tert-Butyl 3-(2-aminoethoxy)propanoate, A new synthetic method of this compound is introduced below., HPLC of Formula: C9H19NO3

Intermediate 214-{5-[2-(2-tei”i-Butoxycarbonyl-ethoxy)-ethylcarbamoyl]-2-hydroxy-phenyl}-4-phen piperidine-l-carboxylic acid ieri-but esterA solution of Intermediate 20 (115 mg, 0.29 mmol), Intermediate 18 (60 mg, 0.32 mmol) and DIPEA (111 mu^, 0.64 mmol) in DMF (5 mL) was treated dropwise with a solution in DMF (1 mL) of HATU (122 mg, 0.32mmol). The reaction mixture was stirred at RT for 3 h then partitioned between water and EtOAc, and the organic extract was further washed with water, dried (Na2S04), filtered and concentrated in vacuo. The crude product was purified by chromatography eluting with 0-50% EtOAc in cyclohexane (90 mg, 78 %).LCMS (Method 2): Rt 4.69 min, m/z 569 [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; ASTRAZENECA AB; PULMAGEN THERAPEUTICS (SYNERGY) LIMITED; DONALD, David, Keith; JENNINGS, Andrew, Stephen, Robert; RAY, Nicholas, Charles; ROUSSEL, Fabien; SUTTON, Jonathan, Mark; TISSELLI, Patrizia; WILSON, Michelle; WO2011/48409; (2011); A1;,
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Ester – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 10259-22-0, name is Ethyl 3-methoxybenzoate, 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 10259-22-0, category: esters-buliding-blocks

General procedure: Hydrazides (30-58) were synthesized by one pot conventionalmethod24 Benzoic acid or its derivative (10 mmol) was dissolvedin ethanol (20 mL). Sulfuric acid (3 N, 2 mL) was added and thereaction contents were refluxed for six hours. The reaction wasmonitored with TLC. After the completion of the reaction, the reactionmixture was neutralized by adding solid NaHCO3, and filteredto remove excess of NaHCO3. In the neutralized reaction mixture which contains ethyl ester, hydrazine monohydrate (1.5 mL,3 mmol) was added and refluxed for 3-6 h to complete the reaction.Ethanol and unreacted hydrazine were removed by distillationupto 1/3 volume. The reaction contents were cooled, filteredand recrystallized from methanol to obtain the desired hydrazidecrystals (see Supporting information).

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, Ethyl 3-methoxybenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Mehr-Un-Nisa; Munawar, Munawar A.; Chattha, Fauzia A.; Kousar, Samina; Munir, Jawaria; Ismail, Tayaba; Ashraf, Muhammad; Khan, Misbahul A.; Bioorganic and Medicinal Chemistry; vol. 23; 17; (2015); p. 6014 – 6024;,
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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. 120-61-6, name is Dimethyl terephthalate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: Dimethyl terephthalate

Dimethyl terephthalate (h) 10g (51. 5mmol) ethanol, 15 ml, is dissolved in a mixed solvent of chloroform 10 ml, hydrate alkylhydrazine 1 25 therein. Adding 8g (515mmol), 4 is made to circulate heating time. After cooling, the solid is separated by filtration in a reaction solution, using ethanol 10 ml, filter to 2 times after washing, drying under reduced pressure, 10g of compound (i) is obtained.

The synthetic route of 120-61-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JNC Corporation; Sasada, Yasuyuki; Minowa, Tetsuharu; (45 pag.)JP5664479; (2015); B2;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Electric Literature of 106-65-0,Some common heterocyclic compound, 106-65-0, name is Dimethyl succinate, molecular formula is C6H10O4, 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.

Synthesis of 5-Methoxycarbonylmethyl-2-thiouracil (181): A mixture of sodium methoxide (13.5 g, 0.25 mol) in 200 mL of diethyl ether was cooled to 0 00 and it was added slowly to a stirred mixture ofdimethyl succinate 178 (36.5 g, 0.25 mol) and ethyl formate (18.5 g, 0.25 mol). The reaction mixture was stirred at 0 CC for 3 h, and at room temperature overnight. The solvent was evaporated, and the residue was washed thoroughly with petroleum ether resulting intermediate 180. The crude intermediate 180 was dissolved in methanol, and 19 g (0.25 mol) of thiourea was added. The reaction mixture was refluxed overnight. It was filtered, and the solid was washed with methanol. The filtrate was concentrated underreduced pressure. Flash chromatographic purification on a silica gel column resulting in the desired product 181 in 20% yield.

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

Reference:
Patent; MODERNA THERAPEUTICS, INC.; ROY, Atanu; CONLEE, Christopher, R.; DE FOUGEROLLES, Antonin; FRALEY, Andrew, W.; (766 pag.)WO2015/196130; (2015); A2;,
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. 35613-44-6, name is Methyl 2-(2-aminophenyl)acetate, A new synthetic method of this compound is introduced below., SDS of cas: 35613-44-6

Preparation of 1 -(1 -(i-methyl-i ,2-dihydroacenaphthylen- 1 -yl)piperidin-4-yl)indolin-2- one (Compound 23-10)[00381j To a solution of 1 -(i-methyl-i ,2-dihydroacenaphthylen- 1 -yl)piperidin-4-one Compound 23-9 (132.68 mg, 0.5 mmol) and methyl 2-(2-aminophenyl)acetate (247.49 mg, 1.5 mmol) in 15 mL of dichioromethane was added acetic acid (150.0mg, 2.5 mmol). The mixture was stirred for 1.5 h at room temperature. Sodium triacetoxyborohydride (316.5 mg, 1.5 mmol) was added into the mixture and stirred2 h at room temperature. Then the reaction mixture was heated to 30C and stirred overnight. The mixture was washed with water (20 mL x 2), and sat. sodium carbonate (20 mL x 2), brine (20 mL x 2). The organic layer were dried over anhydrous sodium sulfate and evaporated in vacuum to afford the crude product. The crude product was purified by silica gel chromatography (ethyl acetate: petroleum ether = 1: 5 to 1: 2) to obtain 1 -(1 -(1-methyl-i ,2-dihydroacenaphthylen- 1 -yl)piperidin-4-yl)indolin-2- one(Compound 23-10, 101.5 mg, yield 53 %) as a white solid. ESIMS (mlz): 382 [M+H].

The synthetic route of 35613-44-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; FANG, Qun, Kevin; SPEAR, Kerry, L.; CAMPBELL, Una; WO2014/106238; (2014); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics