Category: 102-49-8

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. 102-49-8, name is 3,4-Dichlorobenzylamine, A new synthetic method of this compound is introduced below., Application In Synthesis of 3,4-Dichlorobenzylamine

A solution of 1.0 g of 2-amino-5-nitronicotinic acid and 0.96 g of carbonyldiimidazole (CDI) in 10 mL of DMF was stirred for 1 h. Then 1.0 g of 3,4-dichlorobenzylamine was added and the mixture stirred at room temperature for 1 h. The mixture was diluted with 100 mL of water. Yellow precipitate of 2-amino-N-(3,4-dichlorobenzyl)-5-nitronicotinamide was formed, which was filtered and dried under high vacuum to be used in the next step without further purification.

The synthetic route of 102-49-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Koltun, Dmitry; Parkhill, Eric; Boze, Melanie; Zablocki, Jeff; Vasilevich, Natalya; Mayboroda, Elena; Glushkov, Andrei; Cole, Andrew; Chisholm, Jeffrey; US2008/255161; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 102-49-8, A common heterocyclic compound, 102-49-8, name is 3,4-Dichlorobenzylamine, molecular formula is C7H7Cl2N, 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.

To a mixture of 0.5 g (2.7 mmol, 1.0 eq.) of 5-nitroanthranilic acid, 0.5 g (3.3 mmol, 1.2 eq.) of HOBt monohydrate and 0.63 g (3.3 mol, 1.2 eq.) of EDC in 30 mL of CH2Cl2 was added 0.4 mL (3.0 mmol, 1.1 eq.) 3,4-dichlorobezylamine and the mixture stirred at room temperature for 2 hours. The mixture was diluted with 40 mL of sat. NH4Cl solution. The organic phase was dried (NaSO4) and the solvent removed in vacuo. The residue was dried under high vacuum to provide N-(3,4-dichlorobenzyl)-2-amino-5-nitrobenzamide

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; Koltun, Dmitry; Parkhill, Eric; Boze, Melanie; Zablocki, Jeff; Vasilevich, Natalya; Mayboroda, Elena; Glushkov, Andrei; Cole, Andrew; Chisholm, Jeffrey; US2008/255161; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 102-49-8,Some common heterocyclic compound, 102-49-8, name is 3,4-Dichlorobenzylamine, molecular formula is C7H7Cl2N, 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: Following the similar procedures as for compound 13a gave compound13b, white solid, 55percent. 1H NMR (400 MHz, CDCl3) delta 8.10 (d,J=5.1 Hz, 1H), 7.43 (d, J=1.8 Hz, 1H), 7.37 (d, J=8.2 Hz, 1H),7.21?7.15 (m, 1H), 6.84 (d, J=5.1 Hz, 1H), 4.79 (t, J=5.6 Hz, 1H),4.65?4.59 (m, 2H), 3.78?3.68 (m, 1H), 3.62?3.53 (m, 2H), 3.21 (t,J=6.3 Hz, 2H), 3.05?2.95 (m, 2H), 2.82 (s, 3H), 2.78 (s, 3H), 2.58 (t,J=6.9 Hz, 2H), 2.43?2.33 (m, 2H), 2.08?1.98 (m, 4H), 1.87?1.76 (m,4H), 1.72?1.61 (m, 2H). 13C NMR (126 MHz, CDCl3) delta 169.41, 154.57,146.52, 144.37, 140.39, 132.47, 130.98, 130.44, 129.56, 127.05,114.53, 112.28, 55.59, 54.97, 53.01, 46.27, 45.72, 44.85, 38.50, 29.69,28.71, 28.56, 26.62, 22.37. HRMS (ESI): calcd for C26H36Cl2N5O3S [M+H]+: 568.1910; found 568.1898. Retention time 2.35 min,>97percentpure.

The synthetic route of 102-49-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Qin, Li-Huai; Wang, Zhi-Long; Xie, Xin; Long, Ya-Qiu; Bioorganic and Medicinal Chemistry; vol. 26; 12; (2018); p. 3559 – 3572;,
Chloride – Wikipedia,
Chlorides – 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. 102-49-8, name is 3,4-Dichlorobenzylamine, A new synthetic method of this compound is introduced below., HPLC of Formula: C7H7Cl2N

General procedure: Compounds 1?6 were prepared according to conventional organic synthesis methods. 3-Chloropyrazine-2-carboxamide (1.27 mmol) was dissolved in THF (20 mL) in a round bottom flask and after that treated with two equivalents of the corresponding benzylamine and an equimolar amount of triethylamine. The reaction was conducted with continuous stirring and heating (70 ¡ãC) under reflux in an oil bath for 15 h. Compounds 7?15 were synthesised using a microwave reactor with a focused field. 3-Chloropyrazine-2-carboxamide (1.27 mmol) was put into a thick-walled tube together with the corresponding benzylamine (2.54 mmol), pyridine (1.27 mmol), methanol (approx. 5 mL) and a magnetic stir bar and then sealed with a special cap. The reaction parameters were set according to the previously published paper as follows?140 ¡ãC, 30 min, 200 W [29]. Reaction progress was checked by TLC (hexane:ethyl acetate?1:1). Regardless of the synthesis method used,all reaction mixtures were adsorbed on silica and subjected to preparative flash chromatography (hexane and ethyl acetate, gradient elution, detection wavelengths 260 nm and 280 nm). Products were recrystallized from ethanol or ethanol and water if necessary. All final substances were chemically characterized (1H-NMR, 13C-NMR, IR, melting point and elemental analysis).

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:
Article; Jandourek, Ondrej; Tauchman, Marek; Paterova, Pavla; Konecna, Klara; Navratilova, Lucie; Kubicek, Vladimir; Holas, Ondrej; Zitko, Jan; Dolezal, Martin; Molecules; vol. 22; 2; (2017);,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 102-49-8, 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. 102-49-8, name is 3,4-Dichlorobenzylamine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A solution of the 3-cyclohexene-1-carboxaldehyde (375 mg, 3.40 mmol, 1 eq) in 1,2-dichloroethane (8 mL) was treated with the 3,4-dichlorobenzylamine (898 mg, 5.10 mmol, 1.5 eq) and the mixture stirred at rt for 3 hr. Sodium triacetoxyborohydride (1.01 g, 4.77 mmol, 1.4 eq) was then divided into two portions and added to the solution at half-hour intervals, and the solution was left to stir for 18 hr. The reaction mixture was quenched using saturated sodium bicarbonate solution (30 mL) and extracted with ethyl acetate (30 mL). The aqueous layer was further extracted with ethyl acetate (2 x 30 mL) and the combined organic layers were dried over magnesium sulfate, concentrated in vacuo and purified by column chromatography eluting with dichloromethane: methanol (98:2) to yield the product as a pale yellow oil (543 mg, 59percent).

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

Reference:
Article; Brear, Paul; North, Andrew; Iegre, Jessica; Hadje Georgiou, Kathy; Lubin, Alexandra; Carro, Laura; Green, William; Sore, Hannah F.; Hyvoenen, Marko; Spring, David R.; Bioorganic and Medicinal Chemistry; vol. 26; 11; (2018); p. 3016 – 3020;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 102-49-8, name is 3,4-Dichlorobenzylamine, belongs to chlorides-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 102-49-8, Quality Control of 3,4-Dichlorobenzylamine

General procedure: Compounds 5a?7a, 9a?11a, and 13a were synthetized using a microwave reactor with a focusedfield. Corresponding N-benzyl-3-chloropyrazine-2-carboxamide (0.6 mmol) was dissolved in methanol(3 mL) and appropriate benzylamine (1.8 mmol, 3 equiv.), along with pyridine (40 mg, 0.6 mmol,1 equiv.) as a base, were added. Our previous observations revealed that triethylamine (TEA) as a basecannot be used for microwave reactions. During the procedure, TEA is partially decomposed (probablyto diethylamine and similar species, which may act as undesired nucleophiles in the dehalogenationreaction). The use of pyridine as the base combined with benzylamines was experimentally verifiedin previous projects [18]. Conditions for synthesis were 150¡ãC, 30 min, and 100 W. The progressof the reactions was monitored by TLC in system hexane/ethyl acetate 1:1. The reaction mixturewas adsorbed on silica by removing the solvents in vacuo and the product was purified by flashchromatography using gradient elution with ethyl acetate (0?100percent) in hexane. Products 7a and 10awere recrystallized from EtOH/H2O.

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

Reference:
Article; Semelkova, Lucia; Jand’ourek, Ond?ej; Kone?na, Klara; Paterova, Pavla; Navratilova, Lucie; Trejtnar, Franti?ek; Kubi?ek, Vladimir; Kune?, Ji?i; Dole?al, Martin; Zitko, Jan; McPhee, Derek J.; Molecules; vol. 22; 3; (2017);,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 102-49-8, name is 3,4-Dichlorobenzylamine, belongs to chlorides-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 102-49-8, SDS of cas: 102-49-8

General procedure: Triethylamine (0.3643 g, 3.6 mmol) was added to a solution of the appropriate alkylamine or substituted benzylamine 5a-l (3 mmol) in dichloromethane (7.5 mL), and the reaction mixture was stirred for 5 min at room temperature, then 2-chloroacetyl chloride (0.3857 g, 3.6 mmol) was added dropwise to this reaction mixture at 0 C and stirred for 15 min at room temperature. After completion of the reaction, the solvent was evaporated under reduced pressure to afford 6a-l. KI (0.5976 g, 3.6 mmol) and CTAB (98.40 mg, 7.5% mmol) were added to a solution of the crude product 6a-l in acetone (30 mL) and maintained stirring at reflux for 2 h to afford 7al. K2CO3 (0.2073 g, 3 mmol) was added to a solution of scopoletin (0.3843 g, 2 mmol) in acetone (30 mL), and the reaction mixture was stirred at refluxed for 30 min. Then crude intermediates 7a-l were added into the mixture and maintained reflux for 8-12 h (the reaction progress was monitored by TLC with UV detection). After cooling the reaction and filtration, the solvent was evaporated under reduced pressure, and the residue was dissolved in ethyl acetate, washed with saturation sodium bicarbonate, and saturation salt solution successively, dried over anhydrous sodium sulfate, evaporated under reduced pressure to give the target crude products. The crude products were purified by column chromatography using petroleum ether/ethyl acetate from 6:1 to 2:1 as the gradient eluent system to yield the products 26-37.

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

Reference:
Article; Luo, Jinxiang; Lai, Ting; Guo, Tao; Chen, Fei; Zhang, Linli; Ding, Wei; Zhang, Yongqiang; Molecules; vol. 23; 5; (2018);,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 102-49-8, A common heterocyclic compound, 102-49-8, name is 3,4-Dichlorobenzylamine, molecular formula is C7H7Cl2N, 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.

General procedure: A mixture of acid 6 (0.5 g, 1 mmol), EDCI (0.21 g, 1.1 mmol), and HOBt (0.15 g, 1 mmol) in dry CH3CN (10 mL) was stirred at room temperature for 30 min and then treated with the benzyl amine 7a (0.11 mL, 1 mmol). The mixture was stirred at room temperature for an additional 24 h. Then the solution was evaporated to dryness in vacuum. The residue was dissolved in ethyl acetate (20 mL) and washed sequentially with brine (2 .x. 5 mL), 10percent aqueous sodium carbonate (2 .x. 5 mL), 10percent aqueous citric acid (2 .x. 5 mL), and water (2 .x. 5 mL). The organic layer was dried over anhydrous sodium sulfate. Concentration of the dried extract yielded an oily residue, which was crystallized (CH2Cl2/n-C6H14) to give pure 8a amide in 27percent yield.

The synthetic route of 102-49-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Fallah-Tafti, Asal; Foroumadi, Alireza; Tiwari, Rakesh; Shirazi, Amir Nasrolahi; Hangauer, David G.; Bu, Yahao; Akbarzadeh, Tahmineh; Parang, Keykavous; Shafiee, Abbas; European Journal of Medicinal Chemistry; vol. 46; 10; (2011); p. 4853 – 4858;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 102-49-8, 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 102-49-8 as follows.

5.1.2.5 (2r)-N1,N3-Bis(3,4-dichlorobenzyl)-2-nitrocyclohexane-1,3-diamine (7d) 3,4-Dichlorobenzylamine (221 mg, 1.3 mmol) was added to a solution of nitrodiol 6 (101 mg, 0.6 mmol) in H2O (5 mL) and the suspension was stirred overnight at rt. A few drops of CH3OH were added and the mixture was stirred at rt for another 24 h. The mixture was cooled to -6 ¡ãC for a few days. The resulting precipitate was collected by filtration and dried. Colorless solid, mp 92 ¡ãC, yield 258 mg (86percent). C20H21CI4N3O2 (477.2). Rf = 0.78 (CH3OH). 1H NMR (CDCl3): delta (ppm) = 1.08 (qd broad, 2J = 3J = 12.6 Hz, 3J = 3.6 Hz, 2H, 4-Ha, 6-Ha), 1.29 (qt, 2J = 3J = 13.2 Hz, 3J = 3.2 Hz, 1H, 5-Ha), 1.81 (dquint, 2J = 13.8 Hz, 3J = 3.3 Hz, 1H, 5-He), 2.16 (dq, 2J = 13.1 Hz, 3J = 3.4 Hz, 2H, 4-He, 6-He), 3.00 (td, 3J = 11.1 Hz, 3J = 4.1 Hz, 2H, 1-H, 3-H), 3.65 (d, 2J = 13.7 Hz, 2H, Ph-CH2), 3.81 (d, 2J = 13.7 Hz, 2H, Ph-CH2), 4.17 (t, 3J = 10.4 Hz, 1H, 2-H), 7.08-7.12 (m, 2H, Ph-H), 7.33-7.38 (m, 4H, Ph-H). Signals for the NH-protons are not visible in the 1H NMR spectrum. IR: (cm-1) = 3329 (m, nu (N-H)), 1557 (s, nu (NO2)), 1359 (m, nu (NO2)), 820 (m, out-of-plane (Ar-H)). MS (EI): m/z (percent) = 477 (M+, <1), 174 (C7H5Cl2NH+, 56), 159 (C7H5Cl2+, 100). According to the analysis of related databases, 102-49-8, the application of this compound in the production field has become more and more popular. Reference:
Article; Bourgeois, Christian; Werfel, Elena; Schepmann, Dirk; Wuensch, Bernhard; Bioorganic and Medicinal Chemistry; vol. 22; 13; (2014); p. 3316 – 3324;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics