Tag: M.W=100-200

Related Products of 6276-54-6,Some common heterocyclic compound, 6276-54-6, name is 3-Chloropropan-1-amine hydrochloride, molecular formula is C3H9Cl2N, 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.

Compound 8: 3-Chloropropylamine HCl (6.5 g, 0.05 mol) and sodium azide (10 g, 0.15 mol) were dissolved in 50 mL water. The reaction proceeded at 80 C. for 48 hours. 10 N NaOH (6 mL) was then added, and the product was extracted with ether and concentrated in vacuo. Bulb to bulb distillation (Bp=65-75 C. at 20-22 ton) afforded a clear oil (4 g, 80%). 1H-NMR (500 MHz, CDCl3): delta 3.38 (t, J=6.7 Hz, 2H), 2.81 (t, J=6.8 Hz, 2H), 1.73 (p, J=6.8 Hz, 2H).

The synthetic route of 6276-54-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; The Rockefeller University; STELLER, Hermann; SANDU, Cristinel; KELKAR, Anshuman; GANGADHAR, Nidhi; US2013/244325; (2013); A1;,
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. 821-10-3, name is 1,4-Dichlorobut-2-yne, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 1,4-Dichlorobut-2-yne

General procedure: The [2 + 2 + 2] cycloaddition was performed in a similar manner as described in [3]. In brief, to a solution of diyne (1 equiv) and propargyl halide (2 equiv) in dry acetonitrile (5 mL), Mo(CO)6 (5 mol %) was added and the reaction mixture was stirred under MWI conditions for 10-15 min. After completion of the reaction (TLC), the reaction mixture was concentrated at reduced pressure and the crude product was purified by silica gel column chromatography using EtOAc/petroleum ether 5:95 to 30:70 to give the [2 + 2 + 2] cyclotrimerized compounds.

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 821-10-3.

Reference:
Article; Kotha, Sambasivarao; Sreevani, Gaddamedi; Dzhemileva, Lilya U.; Yunusbaeva, Milyausha M.; Dzhemilev, Usein M.; D?yakonov, Vladimir A.; Beilstein Journal of Organic Chemistry; vol. 15; (2019); p. 2774 – 2781;,
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. 6775-78-6, name is 6-Chloroimidazo[1,2-b]pyridazine, A new synthetic method of this compound is introduced below., Recommanded Product: 6775-78-6

478 mg (3.11 mmol) of 6-chloroimidazo[l,2-b]pyridazine were introduced into 10 mL of chloroform under argon and, while cooling in ice, 664 mg (3.73 mmol) of /V-bromo- succinimide were added. After the addition was complete, the reaction mixture was stirred at room temperature overnight. The reaction mixture was then mixed with water and ethyl acetate and, after addition of saturated sodium bicarbonate solution, the phases were separated. The aqueous phase was extracted three more times with ethyl acetate. The combined organic phases were then washed with saturated sodium chloride solution and dried over sodium sulfate. In the final removal of the solvent in vacuo, the desired product was isolated in quantitative yield in the form of an amorphous white solid which was employed without further chromatographic purification in subsequent reactions. H-NMR (CHLOROFORM-d): delta [ppm] = 7.12 (d, 1H); 7.79 (s, 1H); 7.90, (d, 1H).

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; BAYER PHARMA AKTIENGESELLSCHAFT; EIS, Knut; PUeHLER, Florian; ZORN, Ludwig; SCHULZE, Volker; SUeLZLE, Detlev; LIENAU, Philip; WENGNER, Antje, Margret; PETERSEN, Kirstin; BOeMER, Ulf; WO2014/128093; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 13726-14-2, name is 4-Chloro-3-methoxyaniline, molecular formula is C7H8ClNO, 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. category: chlorides-buliding-blocks

General procedure: Compounds 2-19 were synthesized by reductive alkylation ofcommercially available anilines with N-Boc-2-aminoacetaldehydeand benzoylation with 2,4-dichlorobenzoyl chloride with subsequentremoval of Boc-protecting group with 4 N HCl in dioxane.Compound precipitated from hexane/ dioxane reaction mixtureas HCl salt.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 13726-14-2, its application will become more common.

Reference:
Article; Buchynskyy, Andriy; Gillespie, J. Robert; Hulverson, Matthew A.; McQueen, Joshua; Creason, Sharon A.; Ranade, Ranae M.; Duster, Nicole A.; Gelb, Michael H.; Buckner, Frederick S.; Bioorganic and Medicinal Chemistry; vol. 25; 5; (2017); p. 1571 – 1584;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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 7006-52-2 as follows. Computed Properties of C7H8ClN

To a solution of 4-chloro-l-methyl-lH-pyrrolo[3,2-c]pyridine-7-carboxylic acid methyl ester (0.5g) in 1,4-dioxane (5ml) was added 3-chloro-N-methyl aniline (0.629g) and methanesulfonic acid (0.289ml). The mixture was irradiated under microwave conditions at 180¡ãC for 30min. 1,4-dioxane was removed in vacuo and the residue purified by MDAP to give the title compound (350mg). LC/MS [MH+] 330 consistent with molecular formula C17H1635ClN3O2

According to the analysis of related databases, 7006-52-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GLAXO GROUP LIMITED; WO2005/121140; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 2533-69-9,Some common heterocyclic compound, 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, molecular formula is C3H4Cl3NO, 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.

3) A solution of N-(4-methoxybutyl)-o-phenylenediamine in toluene was cooled to 0-10 C., and acetic acid (65.2 g, 1.09 mol) and methyl 2,2,2-trichloroacetimidate (70.3 g, 0.398 mol) were added. After stirring at 0-10 C. for 30 min, the mixture was stirred at 20-30 C. for 3 hr. The reaction mixture was successively washed with 5 w/v % brine (250 mL), a mixed solution of 2N hydrochloric acid/5 w/v % brine (1:1, 250 mL*2), 5 w/v % sodium bicarbonate water (250 mL) and 5 w/v % brine (250 mL). Under a nitrogen stream, magnesium sulfate (25.0 g) was added to the organic layer at 20-30 C., and the mixture was stirred at the same temperature for 30 min. Magnesium sulfate was filtered off and the residue was washed with toluene (100 mL). The filtrate was concentrated under reduced pressure to give the content (150 mL). The concentrated solution was stirred at 20-30 C., the crystals were precipitated, and heptane (750 mL) was added dropwise. The crystallized solution was heated to 40-50 C. and stirred for 30 min. After stirring, the solution was cooled to 0-10 C. and stirred at the same temperature for 2 hr. The precipitated crystals were collected by filtration, washed with toluene-heptane (1:5, 150 mL) and dried under reduced pressure at 40 C. to give 1-(4-methoxybutyl)-2-trichloromethyl-1H-benzimidazole as pale brown crystals (96.5 g, yield 82.9% from o-nitroaniline).1H-NMR (300 MHz, CDCl3) delta: 1.68-1.85 (m, 2H), 1.99-2.17 (m, 2H), 3.37 (s, 3H), 3.48 (t, J=6.1 Hz, 2H), 4.50-4.65 (m, 2H), 7.27-7.49 (m, 4H), 7.82-7.93 (m, 1H).[0086]Anal. Calcd for C13H15Cl3N2O: C, 48.55; H, 4.70; N, 8.71; Cl, 33.07. Found: C, 48.30; H, 4.61; N, 8.74; Cl, 33.30.

The synthetic route of 2533-69-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Kitayama, Masato; US2013/90337; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 78068-85-6, name is 3-Chloro-4-fluorobenzotrifluoride, 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: C7H3ClF4

To a suspension of 3,3′-dihydroxydiphenyl disulfide (1.01 g, 4.03 mmol) and Cs2CO3 (3.3 g, 10 mmol) in DMF (20 mL) was added 3-chloro-4-fluorobenzotrifluoride (2 g, 10 mmol). The reaction was heated at 100 C. overnight. The mixture was then cooled and partitioned between ether (200 mL) and water (200 mL). The aqueous layer was further extracted with ether (2¡Á100 mL). The organic layers were combined, washed with water (1¡Á100 mL), Brine (1¡Á100 mL), dried with anhydrous sodium sulfate, filtered and concentrated. The resulting oil was used in the next step directly.

The synthetic route of 3-Chloro-4-fluorobenzotrifluoride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Ge, Min; He, Jiafang; Lau, Fiona Wai Yu; Liang, Gui-Bai; Lin, Songnian; Liu, Weiguo; Walsh, Shawn P.; Yang, Lihu; US2007/265332; (2007); A1;,
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. 2845-89-8, name is 1-Chloro-3-methoxybenzene, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 1-Chloro-3-methoxybenzene

General procedure: Under a N2 atmosphere, KOtBu (102.1 mg, 1.3 equiv) and a so-lution of complex 3a (10e50 mL, 0.01e0.05 mol%, prepared from4.6 mg of complex 3a in 1.0 mL dichloromethane) were added into aSchlenk reaction tube. The tube was sealed and the solvent wasremoved under reduced pressure. Then toluene (0.5 mL), amines(0.84 mmol) and aryl chlorides (0.70 mmol) were successivelyadded. The mixture was stirred vigorously at the specied tem-perature for 3e24 h. Then the solvent was removed under reducedpressure and the residue was puried by ash column chroma-tography (SiO2) to give the corresponding products.

According to the analysis of related databases, 2845-89-8, the application of this compound in the production field has become more and more popular.

Reference:
Article; Zhang, Zhi-Mao; Gao, Yu-Jue; Lu, Jian-Mei; Tetrahedron; vol. 73; 52; (2017); p. 7308 – 7314;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 69957-83-1, 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 69957-83-1 as follows.

To a solution of N-(4-chlorobenzyl)-JV-ethylamine (0.150 g, 0.88 mmol) and {4-[(25)-2,3- diethoxy-3-oxopropyl]phenoxy}acetic acid (0.270 g, 0.91 mmol) in methylene chloride (10 mL) were added iVyV-diisopropylethylamine (0.34 mL, 1.9 mmol) and O-(benzotriazol-l-yl)- EPO tetrafluoroborate (0.320 g, 1.00 mmol) and the reaction mixture was stirred at room temperature overnight. The resulting solution was diluted with methylene chloride (40 mL) and the organic phase was washed with 5% HCl (50 mL), saturated aqueous NaHCO3 (50 mL), and brine (50 mL), dried over Na2SO4, and concentrated in vacuo. 5 Purification on a prepacked column of silica gel (Isolute SPE Column, 50 g/150 mL) with methylene chloride/ethyl acetate 10:1 as the eluent yielded 0.24 g (61%) of a colourless oil.1H NMR (500 MHz, CDCl3): delta 1.05-1.24 (m, 9H), 2.88-3.00 (m, 2H), 3.28-3.42 (m, 3H), 3.60 (m, IH), 3.96 (m, IH)3 4.12-4.20 (m, 2H), 4.56 and 4.58 (2s, 2H, rotamers), 4.64 and 4.73 (2s, 10 2H, rotamers), 6.75 and 6.88 (2d, 2H, rotamers), 7.09-7.20 (m, 4H), 7.24 and 7.30 (2d, 2H, rotamers).

According to the analysis of related databases, 69957-83-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ASTRAZENECA AB; WO2007/8156; (2007); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 5013-77-4, 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. 5013-77-4 name is N-Methyl-2,4-dichlorobenzylamine, 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.

Into a 100-mL 3-necked round-bottom flask purged and maintained with an inert atmosphere of nitrogen, was placed a solution of 2-bromo 1- (3-mtrophenyl)ethanone (2 g, 8 23 mmol, 1 00 equiv), t?ethylamme (3 4 g, 4 00 equiv), (2,4 dichlorophenyl)-N methylmethanamine (1 9 g, 10 05 mmol, 1 20 equiv), 1,4- dioxane (50 mL) The resulting solution was stirred for 2 h at room temperature at which time it was judged to be complete by LCMS The mixture was concentrated under vacuum and the residue was applied onto a silica gel column with ethyl acetate/petroleum ether (1 100-1 50) This resulted in 1 5 g (50%) of 2-((2,4- dichlorobenzyl)(methyl)ammo)-l-(3-nitrophenyl)ethanone as a yellow solid.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, N-Methyl-2,4-dichlorobenzylamine, and friends who are interested can also refer to it.

Reference:
Patent; ARDELYX, INC.; CHARMOT, Dominique; JACOBS, Jeffrey, W.; LEADBETTER, Michael, Robert; NAVRE, Marc; CARRERAS, Chris; BELL, Noah; WO2010/78449; (2010); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics