Month: June 2021

Synthetic Route of 50893-36-2, The chemical industry reduces the impact on the environment during synthesis 50893-36-2, name is 1-Chloroethyl ethyl carbonate, I believe this compound will play a more active role in future production and life.

EXAMPLE 119B 1-(Ethyloxycarbonyloxy)ethyl 4-{N-butyl-N-[(2′-[N-triphenylmethyl-1H-tetrazol-5-yl]biphenyl-4-yl)methyl]amino}pyrimidine-5-carboxylate The compound resulting from Example 119A (1.00 g, 1.5 mmol) was dissolved in anhydrous dimethylformamide (3 mL) and potassium carbonate (616 mg, 4.5 mmol), 1-chloroethyl ethyl carbonate (460 mg, 3 mmol), sodium iodide (450 mg) and triethylamine (5 drops) were added. After stirring at ambient temperature for 30 hours, the reaction mixture was poured into saturated aqueous ammonium chloride and extracted with ethyl acetate. The combined organic extracts were washed with brine, dried over sodium sulfate and sodium carbonate, and concentrated under reduced pressure. Chromatography eluding with ethyl acetate/hexane mixtures provided the title compound as an amorphous solid (470 mg, 40percent).

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, 1-Chloroethyl ethyl carbonate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Abbott Laboratories; US5250548; (1993); A;,
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Related Products of 87661-20-9, The chemical industry reduces the impact on the environment during synthesis 87661-20-9, name is tert-Butyl cyclopropanecarboxylate, I believe this compound will play a more active role in future production and life.

To a solution of diisopropylamine (24.5 ml) in THF (300 ml) was added at -20 C n-butyllithium (1.6 M solution in hexane, 109 ml), the mixture was warmed to 0C for 30 min and cooled to -78 C. The solution was treated with a solution of cyclopropanecarboxylic acid tert-butyl ester (24.8 g, preparation described in St.W. Wright et al, Tetrahedron Lett. 38, 7345 1997) in THF (50 ml) and after stirring for 4 h at -78C a solution of (R)-2-methyl-propane-2-sulfmic acid [l-(2-fluoro-5-nitro-phenyl)-(E)-ethylidene]- amide (50.0g) in THF (50 ml) was added and stirring was continued for 4 h. The mixture was quenched with brine, extracted with ethyl acetate, the organic layer was dried and evaporated. The residue was purified by chromatography over silica using cyclohexane /ethylacetate (4: 1) to give 1 -[(S)- l-(2-fluoro-5-nitro-phenyl)- 1 -((R)-2-methyl-propane-2-sulfinylamino)-ethyl]- cyclopropanecarboxylic acid tert-butyl ester (17.3 g) as a pale brown oil. MS (ESI): m/z = 429.3 [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, tert-Butyl cyclopropanecarboxylate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; BANNER, David; HILPERT, Hans; MAUSER, Harald; MAYWEG, Alexander V.; ROGERS-EVANS, Mark; WO2011/70029; (2011); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Synthetic Route of 6627-89-0, The chemical industry reduces the impact on the environment during synthesis 6627-89-0, name is tert-Butyl phenyl carbonate, I believe this compound will play a more active role in future production and life.

t-Butyl phenyl carbonate (20 mL, 0.11 mole) was added drop-wise to a solution of N-(3-aminopropyl)-1,3-propanediamine (0.05 mole) in anhydrous DMF (50 mL). To this solution was added Et3N (5 mL). The resulting mixture was stirred at room temperature overnight. The mixture was poured into a phosphate buffer (2 L, 0.025 M K2HPO4 and 0.025 M NaH2PO4), and the resulted solution was adjusted to pH 3 with 2 M H2SO4 with vigorous stirring. The mixture was extracted with DCM (2×250 mL) and the organic extracts were discarded. The aqueous layer was basified with aq. 9 N NaOH; and then was extracted with DCM (3×250 mL). The organic extracts were dried over Na2SO4, concentrated under reduced pressure, and then dried under vacuum overnight to give the desired product (15 g, 90% yield). Di-t-butyloxy Triamine (III):To a solution of triamine (II) (0.05 mole) in DMF (50 mL) was added the t-butyl phenyl carbonate (2.3 eq.). The reaction mixture was stirred overnight at room temperature and poured into phosphate buffer (1 L of 0.05 M K2HPO4 and 0.05 M NaH2PO4). The pH was adjusted to 3 with 2 M H2SO4 and extracted with diethyl ether (3×250 mL). The aq. phase was made strongly alkaline with 10 N NaOH and extracted with DCM (4×250 mL). The organic phase was washed with brine, dried over sodium sulphate, and concentrated under reduced pressure to provide the bis protected triamine (III) as a white solid (yield 60%).

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, tert-Butyl phenyl carbonate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Affymax, Inc.; US2009/48147; (2009); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Synthetic Route of 457097-93-7,Some common heterocyclic compound, 457097-93-7, name is Methyl 4-amino-3-(trifluoromethoxy)benzoate, molecular formula is C9H8F3NO3, 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.

c) 4-Benzyloxycarbonylamino-3-trifluoromethoxy-benzoic acid methyl ester To a solution of 4-amino-3-trifluoromethoxy-benzoic acid methyl ester (4.9 g, 20.8 mmol) and NaHCO3 (5.24 g, 62.4 mmol) in dioxane-water 5:1 (90 mL) is added at 0-5 C. benzyl chloroformate (4.4 mL, 31.3 mmol). After addition the reaction mixture is stirred at 25 C. for 16 h. The reaction mixture is diluted with CH2Cl2 and washed with water, dried over MgSO4 and evaporated. The title compound is obtained after purification by flash-chromatography on silica gel (hexane-EtOAc 30:1 to 10:1) as a colorless oil: TLC (hexane-EtOAc 4:1) Rf=0.52; ESIMS [M-H]-=368.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Methyl 4-amino-3-(trifluoromethoxy)benzoate, its application will become more common.

Reference:
Patent; Briard, Emmanuelle; Lueoend, Rainer Martin; Machauer, Rainer; Moebitz, Henrik; Rogel, Olivier; Rondeau, Jean-Michel; Rueeger, Heinrich; Tintelnot-Blomley, Marina; Veenstra, Siem Jacob; US2009/54427; (2009); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

These common heterocyclic compound, 56741-34-5, name is Methyl 5-amino-2-fluorobenzoate, 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. Computed Properties of C8H8FNO2

An aromatic amine 1d-2 (0.20 mmol), a platensimycin acid (0.10 mmol),2-(7-Azobenzotriazole)-N,N,N’,N’-tetramethyluronium hexafluorophosphate (HATU) (0.30 mmol) was added to the reaction flask and 1.0 ml was added.N,N-dimethylformamide, stirring at room temperature; slowly adding triethylamine (0.45 mmol), stirring for 12 hours, rotary evaporationSolvent to obtain a crude product, which is subjected to column chromatography to obtain a platensimycin analog2d-2, yield 43%.

The synthetic route of Methyl 5-amino-2-fluorobenzoate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Changsha Tianci Bio-pharmaceutical Technology Co., Ltd.; Changsha Cihang Pharmaceutical Institute Co., Ltd.; Ha Yao Cihang Pharmaceutical Co., Ltd.; Duan Yanwen; Shen Ben; Huang Yong; Zhu Xiangcheng; Qiu Lin; Tian Kai; (39 pag.)CN107793388; (2018); A;,
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. 29823-21-0, name is Ethyl 8-Bromooctanoate, A new synthetic method of this compound is introduced below., Recommanded Product: 29823-21-0

a) 2-(4-Methoxyphenyl)-4,5-diphenylimidazole (10 g) (J. Org. Chem., 1964, 29, 1926-30) was reacted with sodium hydride (1.7 g) and ethyl 8-bromooctanoate (9.6 g) in a method similar to Example 12. Chromatography on silica gel eluted with chloroform gave 1-(7-ethoxy-carbonylheptyl)2-(4-methoxyphenyl)-4,5-diphenylimidazole (12.9 g, 85%) as an oil.

The synthetic route of 29823-21-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SmithKline Beecham Corporation; The Johns Hopkins University; US5648373; (1997); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Some common heterocyclic compound, 109232-37-3, name is Isobutyl 5-chloro-2,2-dimethylvalerate, molecular formula is C11H21ClO2, 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. category: esters-buliding-blocks

Compound 1-1 (4-chloro-2,5-dimethylphenol) (780 mg, 5.0 mmol), 5-chloro-2,2-dimethylvaleric acid isobutyl ester (1144 mg, 5.2 mmol), TBAI (36.9mg, 0.1mmol), potassium carbonate (1380mg, 10.0mmol) was dissolved in DMF (30mL), and stirred at 90 C overnight. TLC monitors the tendency of discontinuous conversion. The reaction solution is poured into water and the layers are separated. After the aqueous phase is extracted with ethyl acetate, the organic phases are combined, dried over anhydrous sodium sulfate, filtered and the filtrate is concentrated. Compound 1-2 (1.5 g) was isolated by analysis and the yield was 88%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 109232-37-3, its application will become more common.

Reference:
Patent; Beijing Hou Shenyaode Science And Technology Co., Ltd.; Jiao Ning; Yu Siwang; Song Song; Liu Yameng; Yang Simin; (60 pag.)CN110857268; (2020); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Related Products of 40876-98-0, 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 40876-98-0 as follows.

5-Hydroxy-1-methyl-1H-pyrazole-3-carboxylic acid ethyl ester; [Show Image] (1) To a solution of diethyl oxalacetate sodium salt (30.0 g) in toluene (200 ml), acetic acid (200 ml) and methylhydrazine (15 ml) were added and stirred at 100C for 8.5 hours. The reaction mixture was concentrated, and the resulting residue was diluted with saturated aqueous sodium chloride and extracted with AcOEt. The resulting organic layer was dried over MgSO4, filtered and evaporated under reduced pressure to remove the solvent. The resulting solid was washed with Et2O/hexan (Et2O/hexane = 2/1) and dried to give the titled compound (18.8 g, brown powder). 1H NMR (600 MHz, DMSO-D6) delta ppm: 1.25 (t, J=7.1 Hz, 3 H), 3.59 (s, 3 H), 4.16-4.25 (m, 2 H), 5.77 (s, 1 H)

According to the analysis of related databases, 40876-98-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; TAISHO PHARMACEUTICAL CO., LTD; EP1988081; (2008); 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. 924-99-2, name is Ethyl 3-(dimethylamino)acrylate, A new synthetic method of this compound is introduced below., Application In Synthesis of Ethyl 3-(dimethylamino)acrylate

Example 2To a solution of 17.8 g of triethylamine in 50 ml of toluene are added, at room temperature, first 5.7 g of trifluoroacetic acid and then 7.23 g of ethyl dimethylaminoacrylate. 14 g of trimethylacetyl chloride are metered into this solution which is stirred at room temperature for 6 h. The reaction mixture is poured onto 20 ml of water, the organic phase is removed, the organic phase is washed with 20 ml of water, and the combined aqueous phases are extracted once again with 10 ml of toluene. The combined organic phases are concentrated under reduced pressure. This affords 10.7 g (90% of theory) of ethyl 2-(trifluoroacetyl)-3-(dimethylamino)acrylate.

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 CROPSCIENCE AG; US2010/274049; (2010); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Synthetic Route of 1195768-18-3, 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. 1195768-18-3, name is Methyl 3-amino-2-fluorobenzoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To tetrahydrofuran (37.5mL of a) in the 2-fluoro-3-aminobenzoate ( 15.0g, 88.7mmol, 1.0eq.) and saturated aqueous sodium bicarbonate (120mL), and added dropwise allyl chloroformate (12.75g, 106mmol, 1.19eq.).The reaction was slowly warmed to room temperature.When TLC showed complete reaction, it was poured into water (800mL) and extracted with ethyl acetate.Extract was dried over sodium sulfate, filtered, and concentrated under reduced pressure to provide an amber liquid form of methyl 3 – [(allyloxy) carbonyl] amino-2-fluoro-benzoate (24.8 g of, 100% yield)

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

Reference:
Patent; Pulaixike Company; Zhang, Chao; Ibrahim, Prabha N; Nespi, Marika; Shi, Songyuan; Spevak, Wayne; Habets, Gaston G; Burton, Elizabeth A; Hirth, Klaus-Peter; (181 pag.)CN105228983; (2016); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics