Month: August 2021

Reference of 75148-49-1,Some common heterocyclic compound, 75148-49-1, name is 3-Bromobenzaldehyde Diethyl Acetal, molecular formula is C11H15BrO2, 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 2. 3-iodobenzaldehyde diethyl acetal. To a stirred -78 C. solution of 3-bromobenzaldehyde diethyl acetal, prepared as in step 1, (1.0 g, 3.8 mmol) in THF (10 mL) was added n-butyllithium (1.7 mL, 4.25 mmol, 2.5M in hexanes). The cold reaction mixture was stirred 0.5 hours followed by the addition of a THF (5 mL) solution of iodine (1.09 g, 4.25 mmol). The ice bath was removed and the reaction allowed to warm to ambient temperature. Saturated NH4 Cl was added and the mixture diluted with hexanes. The organic layer was washed with brine, dried (MgSO4) and concentrated under reduced pressure to give a residue which was purified by column chromatography on silica gel eluding with 5% ethyl acetate-hexanes to afford 1.0 g of 3-iodobenzaldehyde diethyl acetal.

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

Reference:
Patent; Abbott Laboratories; US5616596; (1997); A;,
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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. 59557-91-4, name is 4-Bromo-2-methoxyaniline belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C7H8BrNO

To a round bottom flask at r.t. containing formic acid (85%, 27 mL, 624.4 mmol) was added acetic anhydride (16 mL, 169.5 mmol) dropwise. The reaction stirred for 45 min. followed by the dropwise addition of a solution of 4-bromo-2- methoxyaniline (9.01 g, 44.6 mmol) in THF (56 mL). The reaction mixture was quenched with ice-water after 23 h and the resulting precipitate was filtered to afford compound 74a (9.20 g, 90%) as a brown solid. 1HNMR (CDCI3, 400 MHz) 8.45 (d, 1H), 8.26 (d, 1H), 7.72 (s, 1H)1 7.11-7.01 (m, 2H), 3.89 (s, 3H); MS (M-NHCOH+1)+ m/z calcd for C7H6BrO+ = 187.0, found m/z = 187.1

The synthetic route of 59557-91-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SCHERING CORPORATION; WO2009/73777; (2009); A1;,
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Adding a certain compound to certain chemical reactions, such as: 6346-09-4, name is 4,4-Diethoxybutan-1-amine, belongs to ethers-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 6346-09-4, Quality Control of 4,4-Diethoxybutan-1-amine

General procedure: To the cooled solution (5-8) of appropriate sulfonyl chloride (20 mmol) and triethylamine (3.5 ml) in dichloromethane (100 ml) 4,4-diethoxybutane-1-amine (3.4 g, 20 mmol) was added. Reaction mixture was stirred at room temperature for 12 h, washed with saturated NaHCO3 solution in water (100 ml). Organic layer was separated, dried over MgSO4 and evaporated to give target compounds 1.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Article; Gazizov, Almir S.; Smolobochkin, Andrey V.; Anikina, Ekaterina A.; Voronina, Julia K.; Burilov, Alexander R.; Pudovik, Michail A.; Synthetic Communications; vol. 47; 1; (2017); p. 44 – 52;,
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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. 109-85-3, name is 2-Methoxyethylamine, A new synthetic method of this compound is introduced below., Formula: C3H9NO

2-Chloro-5-nitropyridine (4.0 g) was stirred with 2-methoxyethylamine (20 mL) at room temperature for 1 h. The reaction mixture was diluted with water (30 mL) and extracted with ethyl acetate (2 x 50 mL), washed with brine (20 mL), dried over sodium sulphate and evaporated under vacuum. The residue was washed with n-pentane (25 mL) to get N-(2- methoxyethyl)-5-nitropyridin-2-amine (4.8 g, 87 %) as yellow 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; GRUeNENTHAL GMBH; FRANK, Robert; BAHRENBERG, Gregor; CHRISTOPH, Thomas; LESCH, Bernhard; WO2013/13815; (2013); A1;,
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Reference of 450-91-9, The chemical industry reduces the impact on the environment during synthesis 450-91-9, name is 4-Fluoro-2-methoxyaniline, I believe this compound will play a more active role in future production and life.

Compound 2 (8.0 g, 43 mmol) was placed in a 500 ml one-necked reaction flask, and concentrated sulfuric acid (100 ml) was added to dissolve the substrate with constant agitation. At -20 C., concentrated nitric acid (6.15 ml, 48 mmol) was slowly added dropwise with stirring, and the reaction mixture was stirred for 5 mins at this temperature. The reaction progress was monitored by TLC. After the substrate was completely consumed, the mixture was poured into ice water. Sodium hydroxide/water solution (150 ml/300 ml) were added slowly to the reaction system which was kept in an ice-water bath at -20 C., and the pH of the mixture was adjusted to 8-9. After the neutralization, the reaction mixture was extracted with ethyl acetate/water system for three times, and the organic layer was separated, washed with water and saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to give compound a1 (8.7 g) which was used directly in the next reaction. Yield: 80%; purity: 100%; MS m/z(ESI): 187.0 [M+H]+; 1H NMR (400 MHz, DMSO-d6): delta 7.34 (d, J=7.8 Hz, 1H), 7.04 (d, J=13.4 Hz, 1H), 5.25 (brs, 2H), 3.90 (s, 3H).

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, 4-Fluoro-2-methoxyaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SHANGHAI HAIYAN PHARMACEUTICAL TECHNOLOGY CO., LTD.; YANGTZE RIVER PHARMACEUTICAL GROUP CO., LTD.; LAN, Jiong; JIN, Yunzhou; ZHOU, Fusheng; HE, Qi; HE, Xiangyu; LV, Qiang; (87 pag.)US2017/57957; (2017); A1;,
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These common heterocyclic compound, 162705-07-9, name is (Z)-2-Methoxy-5-(3,4,5-trimethoxystyryl)aniline, 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: 162705-07-9

General procedure: DCC (0.47 mmol, 1.2 eq.); the N-Fmoc-protected amino acid (0.472 mmol, 1.2 eq) and HOBt·H2O (0.47 mmol, 1.2 eq) were added to a solution of the 30-aminocombretastatin (0.39 mmol, 1 eq) in anhydrous DMF (1.3 mL). The reaction mixture was stirred under N2 atmosphere for 16 h. Then, it was ltered, and the ltrate was poured into a saturated aqueous NH4Cl solution and then extracted with AcOEt (3×15 mL). The combined organic extracts were washed 2 times with water and brine and dried over anhydrous MgSO4. After ltration and evaporation of the solvent under reduced pressure, the resulting residue was chromatographed on silica gel with Hexanes-AcOEt (6:4) to aord the corresponding N-Fmoc-protected derivatives 7 and 9.

The synthetic route of (Z)-2-Methoxy-5-(3,4,5-trimethoxystyryl)aniline has been constantly updated, and we look forward to future research findings.

Reference:
Article; Agut, Rauel; Alberto Marco, J.; Carda, Miguel; Falomir, Eva; Gil-Edo, Raquel; Martin-Beltran, Celia; Murga, Juan; Pla, Alberto; Molecules; vol. 25; 3; (2020);,
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Related Products of 768-70-7,Some common heterocyclic compound, 768-70-7, name is 3-Ethynylanisole, molecular formula is C9H8O, 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.

General procedure: A 1.6 M solution of n-BuLi in hexanes (1.1equiv) was added to a solution of the corresponding terminal alkyne (1.0 equiv) in THF (5 mL per mmol) at -40 C. After stirring for 30min, acetoxy-benziodoxole 6 (1.1equiv) was added in one portion. The mixture was kept at -40 C for 10 min and then allowed to reach room temperature while stirring for 2 h. Then, the reaction mixture was quenched with a saturated solution of NaHCO3 and extracted three times with dichloromethane. After the evaporation of the solvent, the crude product was purified by column chromatography (silica gel; heptanes/EtOAc) to afford the alkyne dimer 7, as well as 13-24, in the reported yields

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

Reference:
Article; Schoergenhumer, Johannes; Waser, Mario; Tetrahedron Letters; vol. 57; 15; (2016); p. 1678 – 1680;,
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Related Products of 53087-13-1, 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. 53087-13-1, name is 1-(Benzyloxy)-3-bromobenzene, This compound has unique chemical properties. The synthetic route is as follows.

A mixture of 1-benzyloxy-2-bromobenzene (12.8 g, 48.7 mmol) and n-butyllithium (55 mmol) in THF (150 mL) was stirred for 20 min at -78 C, treated with tri-iso-propyl borate (34 mL, 147 mmol), stirred for 20 minutes at -78 C, then 30 minutes at ambient temperature. The mixture was reduced in volume by rotary evaporation, diluted with ethyl acetate washed sequentially with 1M HCl (twice), water, and brine, dried (MgSO4) and concentrated to provide a white solid which was triturated with hexanes to provide the title compound as a white powder (7.04 g). MS (DCI/NH3) m/e 246 (M+NH4)+.

The chemical industry reduces the impact on the environment during synthesis 1-(Benzyloxy)-3-bromobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; ABBOTT LABORATORIES; EP1080070; (2006); B1;,
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Application of 115144-40-6, 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. 115144-40-6, name is 3,4-Difluoroanisole belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

3,4-Difluoroanisole was similarly converted to 2,3-difluoro-6-(methoxy)benzyl bromide (Examples 74A, 75A), and 1-fluoro-3-(trifluoromethoxy)benzene converted to 2-fluoro-6-(trifluoromethoxy)benzyl bromide (Examples 77A, 78A). 2-Chloro-6-(trifluoromethoxy)benzyl alcohol (Examples 89A, 90A) was prepared in similar manner, except that lithium diisopropylamide was used in the formylation reaction, rather than n-butyllithium.

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

Reference:
Patent; Pfizer Inc; US6313100; (2001); B1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

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. 59557-91-4, name is 4-Bromo-2-methoxyaniline, A new synthetic method of this compound is introduced below., Product Details of 59557-91-4

Add in 100mL single-mouth bottles85% sulfuric acid (39 mL) and 4-bromo-2-methoxyaniline (5 g, 24.8 mmol),The temperature was lowered to 0-5 C, and cerium nitrate (3.2 g, 26.1 mmol) was added in portions.After the addition, the temperature was reacted for 45 minutes.The reaction solution was poured into iced 50% aqueous sodium hydroxide (100 mL, pH > 8).The temperature was controlled to stir at 5-10 C, filtered, and the filter cake was rinsed with 100 mL of water.drying. The crude product was beaten with 50 mL of n-hexane for 20 min and filtered.The filter cake was dried to give 4.9 g of a yellow solid. Yield: 80.19%.

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; Beijing Purunao Bio-technology Co., Ltd.; Zhang Peilong; Shi Hepeng; Lan Wenli; Song Zhitao; (250 pag.)CN108707139; (2018); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem