Author: Jessica.F

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. 4316-51-2, name is 4-Methoxytriphenylamine, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 4316-51-2

POCl3 (6 mL, 64.17 mmol) was carefully added to a solution of 4-methoxy-N,N-diphenylaniline (10 g, 36.32 mmol), DMF (5 mL, 64.85 mmol) and 50 mL of 1,2-dichloroethane. The mixture was refluxed for 4 h, then cooled to room temperature (r.t.), and poured into a saturated aqueous sodium acetate solution (100 mL). The product was extracted with dichloromethane. The organic layer was dried over anhydrous MgSO4. The solvent was evaporated by a rotary evaporator. The residue was purified by silica gel column chromatography using ethyl acetate: n-hexane (2:3) to give (1) (7.6 g, Yield: 69%). TOF/MS (ESI): found 326.1 (M+Na+). 1H NMR (300 MHz, CDCl3, delta): 9.79 (s, 1H, ArCHO), 7.68-6.89 (m, 14H, ArH), 3.83 (s, 3H, ArOCH3).

According to the analysis of related databases, 4316-51-2, the application of this compound in the production field has become more and more popular.

Reference:
Article; Giang, Ha Ngoc; Kinashi, Kenji; Sakai, Wataru; Tsutsumi, Naoto; Journal of Photochemistry and Photobiology A: Chemistry; vol. 291; (2014); p. 26 – 33;,
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Adding a certain compound to certain chemical reactions, such as: 5414-19-7, name is 1-Bromo-2-(2-bromoethoxy)ethane, 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 5414-19-7, COA of Formula: C4H8Br2O

General procedure: 1,3-Dibromopropane (2.2 Kg, 10.9 mol) was slowly added to a stirred suspension of 264 g magnesium turnings (11 mol)In tetrahydrofuran (17.6 L).Control the dropping rate to maintain the reaction temperature at minus 40 ~ 50 degrees Celsius.After the addition is complete, the mixture is precooled to minus 50 degrees Celsius for two hours at minus 40 to 50 degrees Celsius,And the reaction mixture prepared from 2-chloropyridine was added.Control the dropping rate to maintain the reaction temperature at minus 40 ~ 50 degrees Celsius.After the addition was completed, the temperature was slowly raised to 60 C and stirred for 3 hours.The reaction mixture was concentrated under reduced pressure to 20 liters of n-hexane (20 L).The resulting solid was removed by filtration.Concentration of the filtrate followed by pressure distillation gave the desired target intermediate (1.16 Kg, 62%) as a colorless liquid.

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:
Patent; Zhejiang Xingyue Pharmaceutical Technology Co., Ltd.; Ying Lv; Chen Qingquan; Hu Junbin; (103 pag.)CN104177394; (2017); B;,
Ether – Wikipedia,
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Application of 929-75-9,Some common heterocyclic compound, 929-75-9, name is 1,11-Diamino-3,6,9-trioxaundecane, molecular formula is C8H20N2O3, 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: 0.41 mmol of polyethylene glycol diamine,DIPEA105 mg, 4-fluoro-2- (2,6-dioxopiperidin-3-yl) ethindol-1,3-one,Add DMF 2mL, 90 C for 12 h. Cool to room temperature,Add water 20mL, ethyl acetate extraction,The extract is saturated with saline,Dried over anhydrous magnesium sulfate,Evaporated under reduced pressure,Silica gel column chromatography (methanol: dichloromethane 1; 10)Intermediate 7.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,11-Diamino-3,6,9-trioxaundecane, its application will become more common.

Reference:
Patent; Jilin University; Lu Haibin; Wang Shihui; Li Haiyan; Wang Chunhe; Deng Jiayu; Feng Mingming; Guo Yu; Su Runping; Jin Xiangqun; (26 pag.)CN106543185; (2017); A;,
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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 145903-31-7 as follows. Application In Synthesis of 7-Methoxy-2,3,4,5-tetrahydrobenzo[f][1,4]thiazepine

Experimental Example 4 7-Methoxy-2,3,4,5-tetrahydro-1,4-benzothiazepine (3.0 g), triethylamine (3.1 g) and bromoacetyl chloride (3.2 g) were reacted in the same manner as in Experimental Example 1 to give 4-bromoacetyl-7-methoxy-2,3,4,5-tetrahydro-1,4-benzothiazepine (2.5 g). IR numaxCHCl3 (cm-1): 1640 1 H-NMR(CDCl3, 100 MHz)delta: 2.75-2.94 (2H, m), 3.68-4.18 (4H, m), 3.80 (3H, s), 4.66-4.81 (2H, m), 6.65-7.58 (3H, m).

According to the analysis of related databases, 145903-31-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Kirin Brewery Co., Ltd.; US5416066; (1995); A;,
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Reference of 123652-95-9, 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. 123652-95-9, name is (3-Fluoro-4-methoxyphenyl)methanamine belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

1. Model canadense amide quinones (DCA – CONH – 07) preparation, comprising the following steps:

The synthetic route of (3-Fluoro-4-methoxyphenyl)methanamine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Guangdong University of Technology; Zhao Suqing; Zhang Bingjie; Feng Dongyan; Fang Yinglin; Wu Ke; Ling Huaying; Tan Qiting; Chen Yanting; Yang Yang; Zhao Jiawei; Ma Zhuolin; Hong Weiqian; (24 pag.)CN109651183; (2019); A;,
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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 162705-07-9 as follows. COA of Formula: C18H21NO4

General procedure: The corresponding N-(1-oxyl-2,2,6,6-tetramethyl-4-piperidinyl-oxycarbonyl) amino acids 20a-h (0.47 mmol) were dissolved in 50 mL of anhydrous CH2Cl2 and cooled to 0 C. 1-Hydroxybenzotriazole (HOBt) (0.7 mmol) and EDCI (0.56 mmol) were added, and the mixture was stirred for 30 min at 0 C. Subsequently, 0.39 mmol of compound 3 and finally 2.4 mL of N-ethyl diisopropylamine were added. The mixture was stirred for 16 h at ambient temperature. The solvent was removed under reduced pressure and the residue was purified by flask-column chromatography (gradient elution with mixtures of chloroform/methanol) on silica gel as monitored by TLC. Synthesized target compounds 21a-h were characterized by mp, IR, ESR and HRMS analyses.

According to the analysis of related databases, 162705-07-9, the application of this compound in the production field has become more and more popular.

Reference:
Article; Liu, Ying-Qian; Li, Xiao-Jing; Zhao, Chun-Yan; Nan, Xiang; Tian, Jing; Morris-Natschke, Susan L.; Zhang, Zhi-Jun; Yang, Xiao-Ming; Yang, Liu; Li, Lin-Hai; Zhou, Xing-Wen; Lee, Kuo-Hsiung; Bioorganic and Medicinal Chemistry; vol. 21; 5; (2013); p. 1248 – 1256;,
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These common heterocyclic compound, 14227-17-9, name is 2,4,6-Trimethoxyaniline, 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. COA of Formula: C9H13NO3

Intermediate 4 (100 mg) was added to 3 MI of POCl3 at 0 C. 2,4, 6- TNMETHOXYBENZENAMINE (0.13 g) was added and the reaction mixture was stirred for 3 to 5 days. The ice bath was allowed to melt during the first couple of hours. After that, the POC13 suspension was dropped to 200 ml of vigorously stirred diisopropyl ether. The solid material was filtered off and washed with diisopropyl ether. The residue was immediately stirred in ETOAC/SATURATED aqueous NAHCO3 (1/1) (200 ML) for 1 hour. The EtOAc was dried using brine and NA2SO4 successively and evaporated. The residue was purified by preparative TLC using CH2CI2/MEOH (95/5) as the eluent or by precipitation in CH2CLZ/MEOH. Yield: 0.01 g of compound 36 (8%).

The synthetic route of 2,4,6-Trimethoxyaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JANSSEN PHARMACEUTICA N.V.; ARTS, Theodora, Joanna, Francisca; JANSSEN, Graziella, Maria, Constantina; JANSSEN, Herwig, Josephus, Margareta; JANSSEN, Jasmine, Josee, Werner; JANSSEN, Paul, Peter, Maria; JANSSEN, Maroussia, Godelieve, Frank; WO2004/74266; (2004); A1;,
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Synthetic Route of 22236-10-8, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 22236-10-8 name is 4-(Difluoromethoxy)aniline, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Example 12; 2-ButyI-5-(4-chIorophenyl)-4-{[4-(difluoromethoxy)phenyl]amino}isothiazol-3(2H)-one 1,1-dioxide; 2-Butyl-4-chloro-5-(4-chlorophenyl)isothiazol-3(2H)-one 1,1-dioxide (0.2Og, 0.60mmol) and 4-(difiuoromethoxy)-aniline (0.19Og, 1.20mmol) were mixed in MeCN (2.5mL). The mixture was heated in a microwave reactor at 130 C for 15 mins, then additional 60 mins and then at 140 0C for 15 mins, then additional 30 mins. The mixture was evaporated and the residue was purified by column chromatography (ISOLUTE SI 20 g/70 mL), eluting with heptane, then DCM:heptane (25:75, then 50:50), to give the title compound (0.122g, 45%);

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-(Difluoromethoxy)aniline, and friends who are interested can also refer to it.

Reference:
Patent; ASTRAZENECA AB; WO2006/73363; (2006); A1;,
Ether – Wikipedia,
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Some common heterocyclic compound, 321-28-8, name is 1-Fluoro-2-methoxybenzene, molecular formula is C7H7FO, 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. Quality Control of 1-Fluoro-2-methoxybenzene

The crude product (1.0 g, 7.9 mmol) was dissolved in acetonitrile (15 mL) and N-bromosuccinimide (1.4 g, 8.7 mmol) was added and reacted at 70 C for 3 h. After the reaction was completed, most of the acetonitrile was distilled off, 30 mL of water was added, the mixture was stirred for 10 min and extracted with ethyl acetate (3 × 20 mL). The combined organic phases were dried over anhydrous magnesium sulfate and separated by column chromatography (pure petroleum ether as eluent) The brominated product (intermediate A_2c) was obtained as a light yellow oily liquid (1.4 g, yield 86%) oA-2c: SH (300 MHz; CDCl 3) 7.23-7.16 (2H, m), 6.82 (D, J = 8.7Hz), 3.86 (3H, s); delta (75MuEtazeta; CDC13) 152.3 (d, Jc, F = 249.0Hz), 147.1 (d, 119.6 (d, J = 21.1 Hz), 114.6 (d, J = 2.2 Hz), 111.9 (d, J = 8.2 Hz), 56.4

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 321-28-8, its application will become more common.

Reference:
Patent; Chinese Academy Of Sciences Chemical Institute; Yu Chuyi; Li Yixian; Jia Tengdun; Zhao Xuan; (27 pag.)CN104557654; (2017); B;,
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Related Products of 5467-58-3, A common heterocyclic compound, 5467-58-3, name is 1-Bromo-4-methoxynaphthalene, molecular formula is C11H9BrO, 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.

Under nitrogen conditions,To the magnetic stirrer,thermometer,6.6 g (27.9 mmol) was added to a 250 mL three-necked flask of a condenser.1-bromo-4-methoxynaphthalene,12.0 g (36.3 mmol) of 4-nitrophenyl-2-amino-9,9-dimethylhydrazine,10.6g (167.4mmol) of copper powder,23.1 g (167.4 mmol) of potassium carbonate,7.4 g (27.9 mmol) of 18-crown-6,Then add 57.2 ml of o-dichlorobenzene,Reacting at 170 C for 20 h;The mixture was filtered while hot, and o-dichlorobenzene was distilled off under reduced pressure. The crude product was recrystallized from ethanol and N,N-dimethylacetamide (V:V = 1:2.7) to give 4-nitrophenyl-4. ‘-Methoxynaphthyl-2-amino-9,9-dimethylhydrazine 10.2 g, yield 75%;

The synthetic route of 5467-58-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Jilin University; Chen Chunhai; Su Kaixin; Wang Daming; Sun Ningwei; Zhou Hongwei; Zhao Xiaogang; (24 pag.)CN108929297; (2018); A;,
Ether – Wikipedia,
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