Month: February 2021

Synthetic Route of 73792-08-2, 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. 73792-08-2, name is Methyl 4-amino-2-fluorobenzoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 7Synthesis of 2-cyano-3-(2-fluoro-4-(7-pivaloyl-5H-pyrrolo[2,3-b]pyrazin-2-ylamino)phenyl)-dimethylacrylamideStep 1To a 250 ml three necked round bottom flask, methyl 4-amino-2-fluorobenzoate (2.75 g, 0.0162 mole) was added in anhydrous THF (60 ml) under nitrogen atmosphere and cooled to 0- 5 C. After 15 minutes, 2.0 M solutions of LAH in THF (24.3 ml, 0.0487 mole) was added dropwise and stirred for 10 min. The reaction mixture was allowed to warm up to room temperature and stirred at same temperature for 1 hr. After completion of the reaction, the reaction mixture was cooled to 5 C and quenched with sat. NH4C1 (25 ml) and diluted with water (100 ml) followed by extraction with ethyl acetate. The combined organics were washed with water, dried over sodium sulphate and evaporated to afford brown solid (crude) product which was purified using column purification by eluting the compound with 20% ethyl acetate in hexanes to yield 1.7 g of (4-amino-2-fluorophenyl)methanol.

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 4-amino-2-fluorobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; PRINCIPIA BIOPHARMA INC.; GOLDSTEIN, David Michael; BRAMELD, Kenneth Albert; VERNER, Erik; WO2012/158785; (2012); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Reference of 61367-07-5,Some common heterocyclic compound, 61367-07-5, name is Methyl trans-4-aminocyclohexanecarboxylate hydrochloride, molecular formula is C8H16ClNO2, 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 stirred solution of 6-(5-cyano-1H-pyrazolo[3,4-b]pyridin-1-yl)-4-(cyclopropylamino)nicotinic acid (0.3 g, 0.94 mmol, Intermediate L), methyl (1R,4R)-4-aminocyclohexane-1-carboxylate hydrochloride (0.18 g, 0.94 mmol), HATU (0.54 g, 1.41 mmol) and DIPEA (0.54 mL, 1.41 mmol) in DMF (5 mL) was stirred at rt for 4 h. The reaction mixture was transferred then into ice water and the resulting precipitate was filtered off and dried under vacuum to give methyl (1R,4R)-4-(6-(5-cyano-1H-pyrazolo[3,4-b]pyridin-1-yl)-4-(cyclopropylamino)nicotinamido)cyclohexane-1-carboxylate as an off white solid (0.38 g, 88%). LC-MS (ESI+) m/z 460.2 (

The synthetic route of 61367-07-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Kymera Therapeutics, Inc.; Mainolfi, Nello; Ji, Nan; Kluge, Arthur F.; Weiss, Matthew M.; Zhang, Yi; (1443 pag.)US2019/192668; (2019); A1;,
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. 27007-53-0, name is Methyl 2-bromo-5-chlorobenzoate, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 27007-53-0

Step B. Methyl 5-chloro-2-cyanobenzoate To a solution of methyl 2-bromo-5-chlorobenzoate (1.15 g, 4.6 mmol) in degassed DMF was added zinc cyanide (282 mg, 2.40 mmol) and palladium tetrakis triphenylphosphine (100 mg, 0.086 mmol) and the reaction is stirred at 90C over night. The reaction was partitioned between ethyl acetate and water. The organic was concentrated in vacuo and purified by flash chromatography eluding a gradient to 10 to 25% ethyl acetate in hexane yielding a white solid (methyl 5-chloro-2-cyanobenzoate). H NMR (CDCl3, 400 MHz): delta 8.13 (d, 1H, J=1.83 Hz); 3.09 (d, 1H, J=8.24 Hz); 7.29 (dd, 1H, J=8.34,2.10 Hz); 4.02(s, 3H).

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 27007-53-0.

Reference:
Patent; Selnick, Harold G.; Barrow, James C.; Nantermet, Philippe G.; Williams, Peter D.; Stauffer, Kenneth J.; Sanderson, Philip E.; Rittle, Kenneth E.; Morrissette, Matthew M.; Wiscount, Catherine M.; Tran, Lekhanh O.; Lyle, Terry A.; Staas, Donnette D.; US2002/119992; (2002); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Electric Literature of 5026-62-0, 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. 5026-62-0, name is Sodium 4-(methoxycarbonyl)phenolate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The above titled compound was prepared by the Method E (ArXBC(R10R11): (4-carboxyphenoxy)methyl). R. Compound A (100 mg) was placed in a 8.0 mL, polypropylene filter column fitted with a 2-way polypropylene stopcock. The resin was pretreated with CH2Cl2 (2 x 3 mL). The swollen resin was then deprotected with 50% TFA/CH2Cl2 (3mL, 30min). The resin was rinsed in the following order: CH2Cl2 (2 x 3 mL), CH3OH (2 x 3 mL), CH2Cl2 (2 x 3 mL). Bromoacetic acid (85 mg) and diisopropyl-carbodiimide (80 mg) in DMF (2.0 mL) was added and the mixture was stirred for 1 hr at room temperature. The resin was filtered and washed in the following order: DMF (2 x 3 mL), CH2Cl2 (2 x 3 mL), DMF (2 x 3 mL), respectively. If a Kaiser test on a small quantity of the resin is positive (blue) then ‘repeat the’ coupling procedure until a negative result is obtained. Methyl p-hydroxybenzoate (91 mg) was pretreated with NaH (20 mg) in THF (0.5 mL) and DMF (2 mL) for 1.5 hr. The resulting phenoxide was added to the resin and the mixture was stirred for 2 hr at room temperature. The resin was then filtered and washed in the following order: DMF (2 x 3 mL), CH2Cl2 (2 x 3 mL), THF (2 x 3 mL), respectively. The resulting resin was then dried in vacuum to constant weight. The cleavage of the resin (saponification) was achieved with LiOH/CH3OH/THF (1:6:20). The resin bound material was placed in the polypropylene column and pretreated with THF (3 mL). Then THF (4 mL), CH3OH (1.0 mL) and 2N LiOH (0.390 mL) were added. The mixture was stirred for 15 min and filtered to a clean and pre weighed test tube. The resin was next washed with THF/5% CH3OH (2mL) and the combined filtrates were evaporated. The resulting gum was dissolved in H2O (1 mL). The solution was then acidified with 1N HCl to pH 2.0. The precipitate was centrifuged, washed with water (2 x 5 mL) and dried in vacuum to furnish the compound of Example 12: ESMS (m/z) 529 (M-H)-

The synthetic route of Sodium 4-(methoxycarbonyl)phenolate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TANABE SEIYAKU CO., LTD.; EP1144365; (2004); B1;,
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. 1150566-27-0, name is Ethyl 6-chloroimidazo[1,2-b]pyridazine-3-carboxylate, A new synthetic method of this compound is introduced below., HPLC of Formula: C9H8ClN3O2

[0328] Step 3: To a solution of B7-3 (600 mg, 2.0 mmol) and {2-[4-fluoro-2-(1-hydroxy-ethyl)- phenoxy]-ethyl}-carbamic acid tert-butyl ester (450 mg, 2.0 mmol) in dry THF (40.0 mL) at -78C was added NaH (60%, 80 mg, 2.0 mmol) in portion. The suspension was stirred at -78 C for 4 h and allowed to warm to 0 C and stirred for additional 4 h. The mixture was then put in the freezer at -20 C overnight. LC-MS showed a good conversion to the desired product. The mixture was then quenched with a mixture of ice and iN HC1 and extracted with EtOAc (3 x 20 mL). The organic layer was dried over Na2504, concentrated and purified twice to afford the desired product B7 as a yellow solid (240 mg, 25%):

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; TP THERAPEUTICS, INC.; CUI, Jingrong Jean; LI, Yishan; ROGERS, Evan W.; ZHAI, Dayong; WO2015/112806; (2015); A3;,
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. 62638-06-6, name is Dimethyl cyclohexane-1,3-dicarboxylate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: esters-buliding-blocks

To a solution of dimethyl 1,3-cyclohexanedicarboxylate (11.6 g, 57.9 mmol) in MeOH (58 mL) was added a 1N NaOH solution (58 mL) dropwise over 1 hr at 0 C. The resulting mixture was stirred at 0 C. for 0.5 hrs, and at room temperature for 2 hrs. The mixture was concentrated under reduced pressure, and the residual solution was partitioned between ethyl acetate and water. The aqueous phase was separated, acidified with conc. HCl (15 mL), saturated with NaCl, and then extracted with ethyl acetate. The extract was dried over Na2SO4, filtered and concentrated under reduced pressure to give 3-(methoxycarbonyl)cyclohexanecarboxylic acid as a colorless oil (6.16 g, yield; 57%).

The synthetic route of 62638-06-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bayer Aktiengesellschaft; US6562811; (2003); B1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Some common heterocyclic compound, 2178-24-7, name is Ethyl (2-bromophenyl)acetate, molecular formula is C10H11BrO2, 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. SDS of cas: 2178-24-7

D. o-Bromophenethyl alcohol To a stirred suspension of 106.0 g of lithium aluminum hydride in 3.7 l of anhydrous ether, is added, dropwise, a solution of 780.0 g of ethyl o-bromophenylacetate in 3.1 l of anhydrous ether. The reaction mixture is stirred for about three hours and then heated under reflux for about five hours. The mixture is cooled, then treated dropwise with 800 ml of water, and 1.5 l of 10% aqueous hydrochloric acid. The ether solution is washed, dried, concentrated, and the residue is distilled to give 554.0 g of o-bromophenethyl alcohol, bp. about 130-132 (8mm), nD20 1,5760.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2178-24-7, its application will become more common.

Reference:
Patent; E. R. Squibb & Sons, Inc.; US3957787; (1976); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Some common heterocyclic compound, 2318-25-4, name is Ethyl 3-ethoxy-3-iminopropionate hydrochloride, molecular formula is C7H14ClNO3, 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. Safety of Ethyl 3-ethoxy-3-iminopropionate hydrochloride

The imidate salt 1g2 (1.5 g, 7.65 mmol) was combined with 2-methyl-3-aminoanisole 1ml (1.05 g, 7.65 mmol, 1 eq.) in ethanol (15 mL) under an N2 atmosphere. The reaction mixture was stirred at RT (24 h) and monitored by HPLC. The reaction mixture was concentrated and then ether was added and the mixture filtered. The solids were washed with ether and the combined ether washes concentrated in vacuo. The resulting adduct 1m2 was purified by chromatography (SiO2, 15percent EtOAc/hexanes) to obtain as a yellow oil (2.11 g, 99percent). MS electrospray: (M+H)+; 280 and (M-H)-; 278.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2318-25-4, its application will become more common.

Reference:
Patent; Boehringer Ingelheim International GmbH; US2006/19905; (2006); A1;,
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. 174403-69-1, name is Methyl 4-fluoro-2-methylbenzoate, This compound has unique chemical properties. The synthetic route is as follows., Safety of Methyl 4-fluoro-2-methylbenzoate

Example 146 Preparation of 2-carbomethoxy-5-fluorobenzyl bromide STR222 A suspension of the compound of Example 145 (5.1 g, 30 mmol), N-bromosuccinimide (5.4 g, 30 mmol) and benzoyl peroxide (0.073 g, 0.30 mmol) in carbon tetrachloride (115 mL) was refluxed for 18 h. The reaction mixture was cooled to 0 C., filtered, and the precipitate was washed with diethyl ether. The solvent was removed in vacuo to afford 7.02 g (94% crude yield) of the title compound, contaminated with a small amount of succinimide. Rf =0.48 20% ethyl acetate/hexanes.

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 174403-69-1.

Reference:
Patent; Corvas International, Inc.; US6011158; (2000); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

These common heterocyclic compound, 40876-98-0, name is Sodium 1,4-diethoxy-1,4-dioxobut-2-en-2-olate, 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: Sodium 1,4-diethoxy-1,4-dioxobut-2-en-2-olate

General procedure: A mixture of malononitrile(2) (0.01 mol) and aromatic aldehyde (3) (0.01 mol) in EtOH was heated for 1 h. Next, a mixture of the sodium salt of diethyloxaloacetate (0.01 mol) (1)and hydrazine hydrate (4) in AcOH was added. The solution was heatedat 120omicronC for 15-30 min. After cooling, the precipitated solid was filtered,and recrystallized from EtOH.

The synthetic route of Sodium 1,4-diethoxy-1,4-dioxobut-2-en-2-olate has been constantly updated, and we look forward to future research findings.

Reference:
Article; Gein; Zamaraeva; Slepukhin; Tetrahedron Letters; vol. 55; 33; (2014); p. 4525 – 4528;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics