Chlorides-buliding-blocks

Application of 3972-56-3, These common heterocyclic compound, 3972-56-3, name is 1-tert-Butyl-4-chlorobenzene, 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.

100 ml of 60% nitric acid was added dropwise to 100 ml of 95% sulfuric acid at a temperature of 35C or less, under ice-cooling, to prepare a mixed acid solution. 100 g (0.593 mol) of 4-tert-butylchlorobenzene (A-1) was added dropwise to this mixed acid solution, at a temperature of 30C or less, followed by after-reaction (20 to 25C) for 2.5 hours. The reaction solution was poured into cold water, and it was then extracted with 100 ml of toluene, followed by washing with water, to obtain a toluene solution of (A-2).

The synthetic route of 3972-56-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; FUJI PHOTO FILM CO., LTD.; EP1535898; (2005); A1;,
Chloride – Wikipedia,
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Electric Literature of 2687-12-9, A common heterocyclic compound, 2687-12-9, name is Cinnamyl chloride, molecular formula is C9H9Cl, 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.

EXAMPLE 1Obtaining 2- (3-N,N-diisopropylamine-l-phenylpropyl) -A- carboxyphenol (IVa)(IVa) Diisopropylamine (2.77 1, 19.65 mol) and sodium iodide(16.95 g, 0.13 mol) were loaded onto a solution of cinnamyl chloride (1 kg, 6.55 mol) in ethanol (3 I/kg) at 20/250C. The mixture was heated at internal 80-850C, the reaction conditions being maintained for 3-4 hours until the end of such reaction.The mixture was cooled at 40-450C and distilled to an internal volume of 1.3 1. The mixture was then cooled at 20- 25C, water (4 1) and toluene (3 1) was added and the pH was adjusted to 1.0-1.5. The phases were decanted and dichloromethane (4 1) was loaded onto the aqueous phase, adjusting the pH again to 11.5-12.0. The phases were decanted and the organic phase was washed with water (4 1) . Once the phases were decanted, the organic phase was distilled at atmospheric pressure to an internal volume of 1.3 1 in order to then load heptane (0.5 1) . Again, it was distilled to 1.3 1 and heptane (2 1) was loaded.The suspension which was obtained was filtered by a prelayer, which was washed with heptane (0.5 1) . The filtered organic phase was distilled at atmospheric pressure to an internal volume of 1.3 1.The amine content of the reaction mixture was determined by the potentiometric titration thereof.

The synthetic route of 2687-12-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; RAGACTIVES, S.L.U.; LORENTE BONDE-LARSEN, Antonio; MARTIN PASCUAL, Pablo; LADERAS MUNOZ, Mario; GUTIERREZ FUENTES, Luis Gerardo; WO2011/12584; (2011); A1;,
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Synthetic Route of 2106-02-7,Some common heterocyclic compound, 2106-02-7, name is 2-Chloro-4-fluoroaniline, molecular formula is C6H5ClFN, 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 mixture of (S)-1-(1-(3-chlorophenyl)-2-hydroxyethyl)-3-(1-(2-chloropyrimidin-4-yl)-1H-pyrazol-4-yl)urea (0.02 g, 0.05 mmol), 2-chloro-4-fluoroaniline (0.009 g, 0.6 mmol), potassium carbonate (0.01 g, 0.075 mmol), and dioxane (2 mL) in a glass tube was purged with nitrogen gas for 20 min. Tris(dibenzylideneacetone)dipalladium(0) (0.002 g, 0.0025 mmol) and BINAP (0.003 g, 0.005 mmol) were added to the reaction mixture, which was purged with nitrogen gas for another 15 min. The tube was sealed and heated at 90 C. for 4 hours. Reaction mixture was filtered through Celite, and filtrate was evaporated; residue was suspended in water, and extracted with ethyl acetate. Organic layer was dried over sodium sulfate, evaporated, and the residue was purified by column chromatography over silica gel using 60% ethyl acetate in hexanes as eluent to give (S)-1-(1-(2-((2-chloro-4-fluorophenyl)amino)pyrimidin-4-yl)-1H-pyrazol-4-yl)-3-(1-(3-chlorophenyl)-2-hydroxyethyl)urea (0.003 g, 12%). 1HNMR (400 MHz, CDCl3, plus a few drops MeOD): 8.50 (s, 1H), 8.33 (d, J=5.2 Hz, 1H), 8.27-8.25 (m, 1H), 7.51 (s, 1H), 7.28-7.19 (m, 1H), 7.23-7.12 (m, 3H), 7.12-7.10 (m, 1H) 7.04-6.99 (m, 1H), 6.23 (d, J=6.8 Hz, 1H) 4.87-4.84 (m, 1H), 3.81-3.77 (m, 1H), 3.64-3.61 (m, 1H). LC-MS calcd exact mass 501.09, found m/z 502.3 [M+H]+. HPLC purity 98.17%.

The synthetic route of 2106-02-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Asana Biosciences, LLC; Venkatesan, Aranapakam M.; Thompson, Scott K.; Smith, Roger A.; Reddy, Sanjeeva P.; (166 pag.)US2016/362407; (2016); A1;,
Chloride – Wikipedia,
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Reference of 2770-11-8, These common heterocyclic compound, 2770-11-8, name is 2-(4-Chlorophenoxy)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.

A solution of the aniline (250 mg, 1.14 mmol), l-acetyl-3-indolecarboxaldehyde (107 mg, 0.57 mmol), NaBH(OAc)3 (302 mg, 1.43 mmol) and AcOH (205 mg, 3.42 mmol) in 1,2-DCE (3 ml) was stirred at room temperature for 16 h. The reaction was quenched with a saturated aqueous solution of sodium bicarbonate (5 ml) and extracted with EtOAc (3 x 5 ml). The combined organics were dried (MgSO4), filtered and concentrated in vacuo before purification by flash chromatography (eluant; 8:2 hexane:EtOAc to EtOAc) proceeded to afford the desired product which was recrystallised from EtOAc and hexane to afford a cream solid (174.1 mg, 78%).1H NMR: (CDCl3, 270 MHz): delta 2.56 (3H, s, CH3), 3.77 (IH, br s, NH), 4.47 (2H, br s,CH2), 6.65-7.50 (12H, m, ArH), 8.41 ppm (IH, d, J= 7.9 Hz, ArH). 13C NMR: (CDCl3, 67.93 MHz): 5 24.1, 39.7, 112.1, 117.0, 117.6, 118.5, 119.0, 119.6,120.1, 123.0, 123.7, 125.5, 125.7, 128.0, 129.7, 136.1, 140.0, 143.5, 156.2, 168.6 ppm.LCMS: 1.550 min, (95% MeOH : 5% water at 1.0 ml/min), AP”: 389.20.HPLC: 3.410 min, 95.90% purity, (isocratic, 90% acetonitrile : 10% water at 1.0 ml/min).HRMS (MicroTOF): C23H20ClN2O2 requires 391.1208, found 391.1194. M.Pt. 107-1080C.

Statistics shows that 2-(4-Chlorophenoxy)aniline is playing an increasingly important role. we look forward to future research findings about 2770-11-8.

Reference:
Patent; STERIX LIMITED; WO2009/66072; (2009); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 104-77-8, name is 3-Chloro-N,N-diethylpropan-1-amine, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C7H16ClN

EXAMPLE 17 Methyl 2-(3-diethylamino-propyl)-5-(3,5-dichlorophenylamino)-2H-1,2,3-triazole-4-carboxylate hydrochloride A mixture consisting of 5.8 gm (0.02 mol) of methyl 1-(3,5-dichlorophenyl)-5-amino-1H-1,2,3-triazole-4-carboxylate, 80 ml of absolute dimethylformamide, 0.8 gm of sodium hydride dispersion and 3.0 gm (0.02 mol) of 1-chloro-3-diethylamino-propane was reacted and worked up as in Example 15. 0.9 gm (9.2% of theory) of the desired compound was obtained; melting point 158 C.

According to the analysis of related databases, 104-77-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Boehringer Ingelheim KG; US4505912; (1985); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 67952-93-6, name is 3-Chloro-4-methylbenzylamine, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 67952-93-6

General procedure: Under an Ar atmosphere, to a solution of benzylamine 1a (0.55 mL, 5 mmol) in 20 mL of CH2Cl2, FeCl3 (811 mg, 5.0 mmol) and m-CPBA (2.2 g, 10.5 mmol, 85%) were added successively at 0 C. The reaction mixture was stirred at 0 C for 3h (TLC monitoring) and quenched with saturated aqueous Na2S2O3 (10 mL). Then, 10% NaOH solution (15 mL) and H2O (15 mL) were added and the mixture wasextracted with CH2Cl2. The combined extracts were dried over anhydrous Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel using petroleum ether/ethyl acetate as eluant to give the light yellow liquid product of N,N-dichlorobenzylamine 2a 850 mg (97%).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 67952-93-6.

Reference:
Article; Liu, Jia; Xu, Junchao; Ren, Jiangmeng; Zeng, Bu-Bing; Chemistry Letters; vol. 43; 2; (2014); p. 190 – 192;,
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Application of 2401-24-3, A common heterocyclic compound, 2401-24-3, name is 2-Chloro-5-methoxyaniline, molecular formula is C7H8ClNO, 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.

EXAMPLE 48 4-(2-Chloro-5-methoxyanilino)-6-(methoxymethyl)-2-(2-methyl-1,3-thiazol-4-yl)pyrimidine The title compound was prepared from a mixture of 4-chloro-6-(methoxymethyl)-2-(2-methyl-1,3-thiazol-4-yl)pyrimidine (50 mg, 0.196 mmol) and 2-chloro-5-methoxyaniline (38 mg, 0.196 mmol) similar to Example 13 and isolated as a white solid (33 mg, 45%). 1H NMR (CDCl3): 8.14 (s, 1H), 7.93 (d, J=3.0 Hz, 1H), 7.32 (d, J=8.7 Hz, 1H), 7.22 (s, 1H), 6.86 (s, 1H), 6.64 (dd, J=3.0, 9.3 Hz, 1H), 4.60 (s, 2H), 3.88 (s, 3H), 3.52 (s, 3H), 2.84 (s, 3H).

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; Cytovia, Inc.; US2003/69239; (2003); A1;,
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. 821-10-3, name is 1,4-Dichlorobut-2-yne, A new synthetic method of this compound is introduced below., Quality Control of 1,4-Dichlorobut-2-yne

1,4-Dichloro-2-butyne (16) (1.26 mL, 13.1 mmol) was added to a solution of malonate 15 (2.50 g, 8.73 mmol) and K2CO3 (3.62 g, 26.2mmol) in MeCN (60 mL) at room temperature. The reaction mixture was stirred for 12h at 90 C, and then H2O (30 mL) was added at 0 C. The resultant mixture was extracted with Et2O (30 mL×3), and the combined organic layers were dried over Na2SO4, filtered, and concentrated. The residue was purified by column chromatography on silica gel (30 g, n-hexane/EtOAc 4/1) to afford chloride 18 (2.54 g, 6.81mmol) in 78% yield.

The synthetic route of 821-10-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Masuda, Keisuke; Tanigawa, Masashi; Nagatomo, Masanori; Urabe, Daisuke; Inoue, Masayuki; Tetrahedron; vol. 73; 26; (2017); p. 3596 – 3605;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 4584-46-7,Some common heterocyclic compound, 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride, molecular formula is C4H11Cl2N, 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 mixture of 4-(4,4,5,5-tetramethyl-1 ,3,2-dioxaborolan-2-yl)-1 /-/-pyrazole (100 mg, 0.515 mmol), 2-chloro-A/,A/-dimethylethanamine hydrochloride (82 mg, 0.567 mmol), and Cs2C03 (504 mg, 1.546 mmol) in acetonitrile (2 ml_) was heated at 90 C for 3 d. After cooling to RT, the reaction mixture was partitioned between DCM and water. The aqueous layer was extracted with DCM and the combined extracts were washed (water), dried (MgS04), and concentrated in vacuo to give the title compound (76 mg, 56%) as a colourless oil. LCMS (Method B): RT = 0.61 min, m/z = 266 [M+H]+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Chloro-N,N-dimethylethanamine hydrochloride, its application will become more common.

Reference:
Patent; ALMAC DISCOVERY LIMITED; O’DOWD, Colin; HARRISON, Tim; HEWITT, Peter; ROUNTREE, Shane; HUGUES, Miel; BURKAMP, Frank; JORDAN, Linda; HELM, Matthew; BROCCATELLI, Fabio; CRAWFORD, James John; GAZZARD, Lewis; WERTZ, Ingrid; LEE, Wendy; (304 pag.)WO2018/73602; (2018); A1;,
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. 823-57-4, name is 2-Bromo-5-chloroaniline, A new synthetic method of this compound is introduced below., Recommanded Product: 823-57-4

General procedure: To a solution of 2-bromoaniline (1.0 equiv.) and N,N-diisopropylethylamine (2.4 equiv.) in toluene was added cis-1,4-dichlorobut-2-ene (1.8 equiv.). The mixture was stirred at reflux until complete consumption monitored by TLC. The reaction was cooled to room temperature, diluted with water, and extracted with EtOAc. The combined organic layers were washed with saturated NaCl solution and dried over Na 2 SO 4 . The solvents were removed under reduced pressure, purified by flash chromatography to give the pure or crude desired product 3. The product 3 was dissolved in anhydrous THF, then was cooled to -78 oC, n-BuLi (1.2 equiv., 2.5 mol/L in n-hexane) was added dropwise to the mixture and keep temperature no more than -50 oC, the mixture was stirred for 30 minutes, (COOR3) 2 (1.0-1.2 equiv.) in THF was added dropwise at -78 oC and stirred at -78 oC for 2 h. The reaction was warmed to room temperature slowly, then quenched with saturated NH 4 Cl solution, and extracted with EtOAc. The combined organic layers were washed with saturated NaCl solution and dried over Na 2 SO 4 . The solvents were removed under reduced pressure, purified by flash chromatography to give the desired product 1.

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; Du, Hong-Jin; Lin, Chao; Wen, Xiaoan; Xu, Qing-Long; Tetrahedron; vol. 74; 52; (2018); p. 7480 – 7484;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics