Month: June 2021

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. 23676-08-6, name is Methyl 4-ethoxybenzoate, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 23676-08-6

To a stirred suspension of CuCN (1.8 g, 20.0 mmol) in 50 mL of dry THF at -78 C under argon, a solution of 1-propenylmagnesium bromide (133.2 mmol, 265 mL of 0.5 M solution in THF) was added dropwise. The slurry was stirred for an additional 30 min and then a solution of methyl 4-ethoxybenzoate (6.0 g, 33.3 mmol) in 60 mL of dry THF was added slowly. The stirred reaction mixture was allowed to warm to room temperature overnight. The reaction wasquenched with ice cold saturated aqueous NaH2PO4 (100 mL) and the mixture was extracted with ether (4 × 100 mL). The combined ether extracts were washed with brine (2 × 100 mL), dried (MgSO4), filtered, and evaporated to dryness. The crude homoallylic ketone was purified by silica gel flash chromatography using a gradient of ethyl acetate in hexane as the eluent to give 8 (7.4 g, 95%) as a colorless oil.

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 23676-08-6.

Reference:
Article; Mandal, Pijus K.; Freiter, Eric M.; Bagsby, Allison L.; Robertson, Fredika M.; McMurray, John S.; Bioorganic and Medicinal Chemistry Letters; vol. 21; 20; (2011); p. 6071 – 6073;,
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These common heterocyclic compound, 35179-98-7, name is Chloromethyl ethyl carbonate, 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. Formula: C4H7ClO3

Example 404-((R)-3-(Bis-ethoxycarbonyloxymethoxy-phosphoryl)-2-{[4-((S)-3-methoxy-pyrrolidin-1-yl)-6-phenyl-pyridine-2-carbonyl]-amino}-propionyl)-piperazine-1-carboxylic acid butyl esterA solution of intermediate 22.2 (100 mg) in abs. DMPU (0.3 mL) and NEt3 (68 muL) was stirred for 10 min at RT. Then, chloromethyl ethyl carbonate (650 mg, prepared as described in WO2004092189) and NaI (29 mg) were added at RT, and the reaction mixture was stirred overnight at 50 C. The reaction mixture was diluted with H2O and the aq. phase extracted with toluene. The combined organic layers were dried over Na2SO4 and concentrated to dryness. CC (EA) gave 19 mg of the desired product.LC-MS: tR=0.97 min; [M+H]+: 822.32.

The synthetic route of Chloromethyl ethyl carbonate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Caroff, Eva; Hilpert, Kurt; Hubler, Francis; Meyer, Emmanuel; Renneberg, Dorte; US2011/46089; (2011); A1;,
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Reference of 18595-18-1, The chemical industry reduces the impact on the environment during synthesis 18595-18-1, name is Methyl 3-amino-4-methylbenzoate, I believe this compound will play a more active role in future production and life.

Step 1: Preparation of methyl 1H-indazole-6-carboxylate (A-2) [0301] Methyl 3-amino-4-methylbenzoate (A-1) (5.0 g, 30.2 mmol) was dissolved in AcOH (140 mL). Sodium nitrite (2.1 g, 30.2 mmol) in water (3.5 mL) was added drop-wise to the solution while stirring at 0 C. The ice bath was removed and the mixture was stirred overnight. Solvents were evaporated, and the mixture was diluted with water (80 mL) and extracted with EtOAc (3×30 mL). The combined organics were washed with water and brine (2×200 mL), dried and evaporated to afford 2 (4.4 g), yield 83%. LCMS (ESI): calc’d for C9H8N2O2, [M+H]+: 177. found: 177.

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 3-amino-4-methylbenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Barr, Kenneth J.; Maclean, John K.; Zhang, Hongjun; Beresis, Richard T.; Zhang, Dongshan; Andresen, Brian M.; Anthony, Neville J.; Lapointe, Blair T.; Sciammetta, Nunzio; US2015/191434; (2015); 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. 426-65-3, name is Ethyl Pentafluoropropionate, A new synthetic method of this compound is introduced below., Recommanded Product: 426-65-3

Ethyl pentafluoropropylenate (14.6 g) and hydrazine monohydrate (3.6 g) were refluxed in tetrahydrofuran (300 ml) for 1 hour. After cooling to room temperature, trifluoroacetamidine (10.0 g) was added dropwise to the mixture and it was refluxed for 3 hours. After finishing the reaction, satu- rated aqueous solution of sodium hydrogen carbonate was added thereto and the mixture was extract- ed with ethyl acetate. After drying the organic layer with anhydrous magnesium sulfate, the solvent was distilled off to obtain crude 3-pentafluoroethyl-5-trifluoromethyl-lH- (1, 2, 4)-triazole (7.9 g).

The synthetic route of 426-65-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER CROPSCIENCE AG; WO2005/95351; (2005); A1;,
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Reference of 61367-07-5, 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. 61367-07-5, name is Methyl trans-4-aminocyclohexanecarboxylate hydrochloride belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

(3) A suspension of the compound obtained in the above step (2) (10 g), 1,5-diiodopentane (9.2 mL) and sodium carbonate (16.4 g) in tetrahydrofuran (300 mL)/N,N-dimethylacetamide (60 mL) was stirred at 70 C for 20 hours. The reaction mixture was concentrated in vacuo and the residue was dissolved in ethyl acetate/water. The organic layer was separated and washed successively with water and brine, dried over sodium sulfate and concentrated in vacuo. The resultant residue was purified by a column chromatography on NH-silica gel (Solvent; ethyl acetate/n-hexane = 1: 5) to give methyl trans-4-(1-piperidyl)cyclohexanecarboxylate (10.17 g). MS(APCI)m/z; 226 [M+H]+

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 trans-4-aminocyclohexanecarboxylate hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; TANABE SEIYAKU CO., LTD.; EP1772454; (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. 56741-34-5, name is Methyl 5-amino-2-fluorobenzoate, A new synthetic method of this compound is introduced below., Product Details of 56741-34-5

A solution of 5-amino-2-fluorobenzoic acid methyl ester (340 mg, 2 mmol), 6-mercaptonicotinic acid (310 mg,2 mmol), and EEDQ (500 mg, 2 mmol) in anhydrous DMF (4 mL) was stirred overnight under N2 at room temperature,2-Bromomethylphenyl boronic acid (428 mg, 2 mmol) was added to the reaction mixture for another 16 hours at roomtemperature. The solvent was then removed by rotary evaporation, and the residue dissolved in EtOAc (25 mL), Theorganic layer was washed with H2O, 10% Na2CO3, H2O, 1 N HCl, H2O, brine, and dried over Na2SO4. The organic layerwas filtered and evaporated to yield 597 mg (68%) of the methyl ester derivative as a light yellow solid. The methyl esterintermediate (200 mg, 0.45 mmol) was dissolved in MeOH (6 mL) and 1 N NaOH (1.35 mL) was added to the reactionmixture. The reaction was stirred for 16 hours at room temperature. The MeOH was removed by rotary evaporation,and the resulting solution acidified with IN BCl. The resulting solid was washed and dried to yield 87 mg (45%) as anoff white solid. ESI-MS m/z = 426.93 [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; Syntrix Biosystems, Inc.; Maeda, Dean Y.; Zebala, John A.; EP2942346; (2015); A1;,
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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. 110661-91-1, name is tert-Butyl 4-bromobutanoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of tert-Butyl 4-bromobutanoate

N-[cis-3-[(4-chlorophenyl)sulfonyl]-3-(2,5-diflupsilonorophenyl)cyclobutyl]-l .1,1- trifluoromethanesulfonaniide (190 mg, 0.388 mmol) was added to DMF (1.1 mL) and treated with potassium carbonate (59 mg, 0.427 mmol), tert -butyl 4-bromobutanoate (95 mg, 0.427 mmol). The mixture was heated to 80 C and stirred for 16 hours. The reaction was cooled to ambient temperature, diluted with ethyl acetate, and washed with 1/2 saturated brine solution twice. The organic layer was dried over anhydrous magnesium sulfate, filtered then concentrated in vacuo. The residue was purified by MPLC ( 0-30 % EtOAc:Hept) to give the title compound. MS: cal’d 654 (M Na+), exp 654 (M Na+)

The synthetic route of 110661-91-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK SHARP & DOHME CORP.; MILLER, Thomas; WO2010/68564; (2010); 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. 154825-97-5, name is Methyl 2-(4-bromophenyl)-2,2-dimethylacetate, A new synthetic method of this compound is introduced below., category: esters-buliding-blocks

Preparation of Intermediate 1 -bromo-4-(1 -methoxy-2-methylpropan-2-yl)benzene (1AA- 11; Methyl 2-(4-bromophenyl)-2-methylpropanoate (23.5g, 86.6mmol) in tetrahydrofuran (175ml_) was cooled to -78C. Lithium aluminum hydride (100 ml. of 1.0 M solution) added slowly over 45 minutes and stirred for 3 hours at cold temperature. Reaction solution was slowly diluted with ethyl acetate and stirred for 10 minutes. 1 M hydrochloric acid was slowly added drop wise to reaction mixture. Diethyl ether (20OmL) added and layers separated. Organic washed with 1 M hydrochloric acid, brine, dried over sodium sulfate, filtered and concentrated to give 2-(4-bromophenyl)-2- methylpropan-1-ol (20m, 100%) as a white solid.

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; PFIZER INC.; ASPNES, Gary, Erik; DOW, Robert, Lee; MUNCHHOF, Michael, John; WO2010/86820; (2010); A1;,
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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 2216-92-4 as follows. SDS of cas: 2216-92-4

N-phenylglycine ethyl ester (781 mg, 4.3 [MMOL),] 4-chlorobenzyl chloride (690 mg, 4.3 [MMOL)] and sodium iodide (64 mg) were dissolved in toluene (7 mL) under argon. The reaction was heated in a graphite bath at 80 [C] for 24 h. After cooling to room temperature, the reaction was diluted with ethyl acetate and washed with [1 M HCI FOLLOWED] by brine. The solution was dried over MgS04, filtered, and concentrated in vacuo. Purification of the resultant oil by flash chromatography (10: 1 hexanes/EtOAc) afforded the title compound as a green oil (669 mg, 51 %). MS (ES+) [M/Z 304 (MH+).]

According to the analysis of related databases, 2216-92-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; PHARMACIA CORPORATION; WO2003/99769; (2003); A1;,
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10601-80-6, name is Ethyl 3,3-diethoxypropionate, 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. Application In Synthesis of Ethyl 3,3-diethoxypropionate

4-Chloro-2-nitrobenzaldehyde (3.71 g, 0.02 mol) was dissolved in ethanol (40 ml).Further adding stannous chloride (18.04g, 0.08mol) and ethyl 3,3-diethoxypropionate (9.5g, 0.05mol), and reacting at 90 C for 4 hours, the reaction of the raw materials of the plate is completed; After the solvent was added, ethyl acetate was dissolved, and neutralized to a weak basic with saturated sodium carbonate; filtered, the organic layer was separated, and the aqueous layer was extracted with ethyl acetate, and then the organic layer was combined, and then evaporated to dryness. Ethyl acetate = 10:1, then petroleum ether: ethyl acetate = 5:1) After washing, ethyl 7-chloro-3-quinolinecarboxylate (3.478 g, 74%).

The synthetic route of 10601-80-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Suzhou Kangrun Pharmaceutical Co., Ltd.; Jin Haowen; Xu Weiliang; Xu Weizheng; (8 pag.)CN108484497; (2018); A;,
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