Category: 4584-46-7

Related Products of 4584-46-7, 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 4584-46-7 as follows.

Me2N(CH2)2Cl.HCl (1.77 g, 12 mmol), K2CO3(3.40 g, 25 mmol) and water (8 mL) were added to 31 (1.68 g, 8.2 mmol)in CHCl3 (40 mL). The stirred solution was placed in an oil bath at65C. The temperature was slowly raised to 80C during 65 min and themixture was stirred for 16 h at 80C. The organic phase was separated and thesolvent was evaporated to 25% of its original volume. This solution was combinedwith the aqueous phase and diluted with water and toluene. The organic layerwas separated, washed with water and extracted with aq. HCl (1.0 M). The acidicphase was washed (toluene), cooled to 0C, basified (~pH 12) by addition ofaq. NaOH (4.0 M) and extracted (toluene). The extract was washed (water,brine) and dried. Evaporation gave 32 (1.81 g, 80%) as a white solid: mp108-109 (lit.3 mp 110C); IR numax 3315, 1687; 1HNMR d 1.39 (3 H, t, J = 7.1 Hz, OCH2CH3), 2.35 (6 H, s, NMe2),2.76 (2 H, t, J = 5.8 Hz, Me2NCH2CH2), 4.10 (2 H, t, J = 5.8 Hz, Me2NCH2CH2),4.39 (2 H, q, J = 7.1 Hz, OCH2CH3),6.99 (1 H, dd, J = 8.9, 2.4 Hz, 6-H),7.07 (1 H, d, J = 2.4 Hz, 4-H), 7.12(1 H, dd, J = 2.1, 0.8 Hz, 3-H), 7.28(1 H, d, J = 8.9 Hz, 7-H), 9.30 (1 H,s, NH); 13C NMR d14.32 (OCH2CH3),45.83 (NMe2), 58.38 (Me2NCH2CH2), 60.82 (OCH2CH3), 66.57 (Me2NCH2CH2), 103.67 (4-C), 108.13(3-C), 112.69 (7-C), 117.37 (6-C), 127.74 (2-C), 127.89 (3a-C), 132.42 (7a-C),153.83 (5-C), 162.01 (C=O)

According to the analysis of related databases, 4584-46-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Twum, Elvis A.; Nathubhai, Amit; Wood, Pauline J.; Lloyd, Matthew D.; Thompson, Andrew S.; Threadgill, Michael D.; Bioorganic and Medicinal Chemistry; vol. 23; 13; (2015); p. 3481 – 3489;,
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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 4584-46-7 as follows. HPLC of Formula: C4H11Cl2N

A mixture of 4-(4,4,5,5-tetramethyl-1 ,3,2-dioxaborolan-2-yl)phenol (0.22 g, 1 .00 mmol), 2-chloro-N,N-dimethylethanamine hydrochloride (0.17 g, 1.15 mmol) and cesium carbonate (1.3 g, 4.00 mmol) in tetrahydrofuran (4 mL) was heated at 130 00 for 2 hours under microwave irradiation. After cooling to room temperature the reactionmixture was partitioned between water and ethyl acetate. The organic phase was separated, washed with additional water and brine, dried over sodium sulfate and thesolvent was evaporated to dryness to yield the title compound (254 mg, 86%) as a brownish oil.LRMS (mlz): 291 (M+1).1H-NMR (300 MHz, CDCI3): 1.3 (s, 12H), 2.3 (s, 6H), 2.7 (t, 2H), 4.1 (t, 2H),6.8 – 7.0 (d, 2H), 7.6 – 7.9 (d, 2H).

According to the analysis of related databases, 4584-46-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ALMIRALL, S.A.; BACH TANA, Jordi; PEREZ CRESPO, Daniel; LLERA SOLDEVILA, Oriol; ESTEVE TRIAS, Cristina; TABOADA MARTINEZ, Lorena; WO2015/86693; (2015); A1;,
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Synthetic Route of 4584-46-7, The chemical industry reduces the impact on the environment during synthesis 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride, I believe this compound will play a more active role in future production and life.

(1) 1.52 g (10 mmol) of methyl 4-hydroxybenzoate was dissolved in 40 ml of N,N-dimethylformamide and 2.16 g (15 mmol) of 2-dimethylaminoethyl chloride hydrochloride and 4.15 g (30 mmol) of potassium carbonate were further added. The mixture was heated at 80 C. and stirred overnight. After cooling, water was added to the reaction mixture, the obtained mixture was extracted twice with ethyl acetate, and the extract was washed with brine. The organic phase was dried (Na2 SO4) and the solvent was distilled off. The resulting residue was purified by silica gel column chromatography (chloroform:methanol=70:1 to 15:1 (v/v)) to obtain 0.69 g (3.09 mmol) of methyl 4-(2-dimethylaminoethoxy)benzoate as a pale brown oily substance. Its spectroscopic data are as follows: 1 H-NMR (CDCl3) delta (ppm):2.34 (6H, s), 2.75 (2H, t, J=5.8 Hz), 3.88 (3H, s), 4.1 2 (2H, t, J=5.6 Hz), 6.93 (2H, d, J=9.2 Hz), 7.98 (2H, d, J=9.2 Hz)

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, 2-Chloro-N,N-dimethylethanamine hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Terumo Kabushiki Kaisha; US6069149; (2000); A;,
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Adding a certain compound to certain chemical reactions, such as: 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride, 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 4584-46-7, Safety of 2-Chloro-N,N-dimethylethanamine hydrochloride

The experimental equipment used in this study was a Vapourtec R4/R2+ flow reactor. Stock A: Ginkgolide B (4.4g), acetonitrile (100mL). Stock B: DECH (2.15g), potassium iodide (0.332g), acetonitrile (90mL), water (10mL). Initially, two flows were pumped into micromixer LH 25. Upon mixing together, the mixture entered the packed bed microreactor filled with acid-binding agents. The total volume of the packed bed microreactor was 24.5mL. However, the remaining volume was 4.5mL when the microreactor was filled with calcium carbonate (2.5g). The volumetric flow rate of stock A/B was 0.75mL/min. That is to say, the residence time in the microreactor was 3min. Upon completion at a set temperature for the appropriate residence time, the obtained organic layer was concentrated under vacuum and further purified by column chromatography on silica gel (MeOH/CH2Cl2=1:50). Dimethylaminoethyl ginkgolide B: 1H NMR (DMSO-d6, 300MHz): delta 7.12 (s, 1H), 6.32 (s, 1H), 6.12 (s, 1H), 5.31 (d, 1H, J=3.6Hz), 5.12 (s, 1H), 4.54 (d, 1H, J=7.5Hz), 4.35-4.41 (m, 1H), 4.07 (d, 1H, J=7.2Hz), 3.55-3.59 (m, 1H), 2.81-2.88 (m, 1H), 2.57-2.64 (m, 1H), 2.32 (d, 1H, J=12.6Hz), 2.18 (s, 6H), 2.11-2.12 (m, 1H), 1.83-1.94 (m, 1H), 1.71-1.77 (m, 1H), 1.11 (d, 3H, J=6.9Hz), 1.04 (m, 9H). 13C NMR (DMSO-d6, 300MHz): delta 176.44, 173.02, 170.18, 109.59, 98.40, 92.78, 82.00, 78.62, 74.36, 74.00, 72.19, 67.52, 64.11, 57.44, 48.64, 43.71, 41.62, 40.09, 39.81, 39.53, 39.25, 38.98, 36.57, 31.75, 28.58. HRMS calcd. for C24H33NO10 496.2177 [M+H], found 496.2196.

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; Qin, Yin-Lin; He, Wei; Su, Mei; Fang, Zheng; Ouyang, Ping-Kai; Guo, Kai; Chinese Chemical Letters; vol. 27; 10; (2016); p. 1644 – 1648;,
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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. 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride, A new synthetic method of this compound is introduced below., Product Details of 4584-46-7

To a stirred solution of 2-chloro-N,N- dimethylethan-1 -amine hydrochloride (2.00 g, 13.8 mmol) in DMF (20.0 ml_), at r.t under N2atmosphere, was added sodium azide (2.71 g, 41.7 mmol) portion wise over a period of 5 min. After complete addition the reaction mixture was heated at 60 C for 6 h. The reaction mixture was cooled to r. t and the contents were slowly poured onto water (50 ml.) and extracted with MTBE (2 x 100 ml_). The combined organic extracts were washed with brine (100 ml_), dried over anhydrous Na2S04, filtered and concentrated under vacuum to obtain 2-azido-N, N- dimethylethan-1 -amine.

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; THE SCRIPPS RESEARCH INSTITUTE; EXPANSION THERAPEUTICS, INC.; DISNEY, Matthew; BLIZZARD, Timothy, Allen; RZUCZEK, Suzanne; NDUNGU, John; VACCA, Joseph; JENNINGS, Andy; PUSHECHNIKOV, Alexei; (333 pag.)WO2019/99777; (2019); A2;,
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Reference of 4584-46-7, 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. 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A mixture of 2-(2,4-dimethoxy-benzyl)-4-hydroxy-isoindole-1,3-dione (317 mg, 1.01 mmol), 2-dimethylaminoethyl chloride hydrochloride (160 mg, 1.11 mmol) and potassium carbonate (350 mg, 2.5 mmol) in DMF (4 mL) was heated at 60 C. for 18 hours. The mixture was concentrated in vacuo, taken up in ethyl acetate and extracted twice with 1N hydrochloric acid. The aqueous extracts were made basic with solid potassium carbonate and extracted with ethyl acetate (×2). The combined organic extracts were washed with brine, dried (MgSO4) and concentrated to give the title compound (236 mg, 61%) as an off-white solid. 1H NMR (methanol-d4) 7.73 (1H, t), 7.44-7.40 (2H, m), 7.02 (1H, d), 6.51 (1H, d), 6.42 (1H, dd), 4.72 (2H, s), 4.33 (2H, t), 3.80 (3H, s), 3.76 (3H, s), 2.87 (2H, t), 2.40 (6H, s). MS: [M+H]+ 385.

The synthetic route of 2-Chloro-N,N-dimethylethanamine hydrochloride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTEX THERAPEUTICS LIMITED; US2010/152184; (2010); A1;,
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Application of 4584-46-7, These common heterocyclic compound, 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride, 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.

In a 250 mL three-necked flask, 20 g of 2-dimethylaminochloroethane hydrochloride (139 mmol) was added,150 mL of DMF-H2O mixed solution (v/v: 7:3),10 grams of sodium azide (154 mmol) and a catalytic amount of NaI.The reaction solution was heated to 80 C., incubated for 36 h, and cooled to room temperature.The reaction solution was neutralized with sodium carbonate, and then the pH of the reaction solution was adjusted to 11 with sodium hydroxide.Add 100 mL of ethyl acetate and extract three times with 180 mL of ethyl ether to combine the organic phase.Dry over anhydrous magnesium sulfate, filter, and evaporate the solvent ether under reduced pressure at room temperature.Add 100g to the above residual ethyl acetate solution1-Iodine-1H,1H,2H,2H-perfluorodecane (174 mmol), warmed to 75C, and reacted overnight to precipitate a yellow solid, the supernatant was removed, and the solid was washed three times with ethyl acetate in a vacuum. After drying for 2 days, a fluoromonomer modified by a click functional group was obtained.

The synthetic route of 4584-46-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Guangzhou Keerbo New Materials Technology Co., Ltd.; Hu Jianqing; Peng Kaimei; Deng Jian; Guo Hongwei; (17 pag.)CN107573250; (2018); A;,
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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. 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride, A new synthetic method of this compound is introduced below., Recommanded Product: 2-Chloro-N,N-dimethylethanamine hydrochloride

General procedure: Requisite alkylaminoethyl chloride hydrochloride, chlorobromopropane and cyclopentyl bromide (6.0mmol) were added to a stirred and refluxing slurry of 4-hydroxybenzaldehyde (1.0g, 8.19mmol) in ethyl methyl ketone (C4H8O) (40ml) in the presence of anhydrous potassium carbonate (2.0g, 14.47mmol). The reaction mixture was further refluxed for 6h with continuous stirring. The completion of the reaction was monitored by TLC. On completion, the reaction mixture was cooled, filtered and the solvent was removed under reduced pressure to obtain an oily residue of corresponding aldehyde 3-9, which was used as such for further reaction.

The synthetic route of 4584-46-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Yadav, Rakesh; Bansal, Ranju; Kachler, Sonja; Klotz; European Journal of Medicinal Chemistry; vol. 75; (2014); p. 327 – 335;,
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Electric Literature of 4584-46-7, These common heterocyclic compound, 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride, 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.

A flame-dried two-necked 25 mL round-bottomed flask was charged with cyclic sulfite (1 mmol), Fe3+-clay (100 mg) and dry xylene (5 mL) and stirred under a constant flush of nitrogen. Freshly distilled 2-aminothiophenol (0.9 mmol) was added drop wise, and the reaction mixture was refluxed for 12 h. Crude compound was chromatographed to get cis-(+)-2,3-dihydro-3-hydroxy-2-(4-methoxyphenyl)-1,5-benzothiazepin-4(5H)-one (50% yield). The hydroxy lactam (0.54 mmol) was dissolved in ethyl acetate (5 mL) and 2-(dimethylamino) ethyl chloride hydrochloride (0.694 mmol) was added followed by addition of finely ground K2CO3 (2.16 mmol) and a drop of water. The heterogeneous mixture was stirred at reflux for 12 h. Solvent was removed and the crude product was chromatographed to obtain N-alkylated product (88%).

The synthetic route of 4584-46-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; COUNCIL OF SCIENTIFIC AND INDUSTRIAL RESEARCH; WO2004/58734; (2004); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride, 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 4584-46-7, Product Details of 4584-46-7

To a solution of 4-hydroxy-3-methoxybenzaldehyde (10g) in DMF (500ml) were added potassium carbonate (18.20g)and 2-chloro-N,N-dimethylethylamine hydrochloride (14.08g). The reaction mixture was stirred at 80C for 1 h30min. The suspension was filtrated off and the filtrate was diluted with Et20 and sat. aq. NaCI. The aq. layer was extracted with Et20, the combined org. layers were dried over MgS04, filtrated off and evaporated in vacuo. The crude was purified by CC (Buchi Sepacore, 70g cartridge, solvent A: DCM, solvent B: MeOH, gradient in %B: 2 to 4, flow rate: 20ml/min) to afford 7.3g of a yellow oil. LC-MS (A): tR = 0.60min; [M+H]+: 224.48.

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; ACTELION PHARMACEUTICALS LTD; BUR, Daniel; GRISOSTOMI, Corinna; KIMMERLIN, Thierry; REMEN, Lubos; SIENDT, Herve; VERCAUTEREN, Magali; WELFORD, Richard; (138 pag.)WO2016/177690; (2016); A1;,
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