Tag: M.W=100-200

Related Products of 41789-95-1, These common heterocyclic compound, 41789-95-1, name is 1-(3-Methoxyphenyl)-N-methylmethanamine, 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: Amine (1.2 equiv) and 3-bromotoluene (1 equiv) were added to an aqueous solution of TPGS-750-M-2% (1 mL/mmol). The mixture was degassed by bubbling Argon in through (5 min). NaO-t-Bu (1.5 equiv), of [(allyl)PdCl]2 (1.1%) and cBridp (4.4%) were added together to the previous solution. The mixture was stirred (at 1200 rpm) at 50 C (2-24 h). Volatiles were evaporated and the crude residue was purified by chromatographic column on silica gel using ethyl acetate and cyclohexane as solvent.

Statistics shows that 1-(3-Methoxyphenyl)-N-methylmethanamine is playing an increasingly important role. we look forward to future research findings about 41789-95-1.

Reference:
Article; Salome, Christophe; Wagner, Patrick; Bollenbach, Maud; Bihel, Frederic; Bourguignon, Jean-Jacques; Schmitt, Martine; Tetrahedron; vol. 70; 21; (2014); p. 3413 – 3421;,
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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. 7664-66-6, name is 4-Isopropoxyaniline, A new synthetic method of this compound is introduced below., HPLC of Formula: C9H13NO

General procedure: 2-Hydroxynaphthalene-1-carboxylic acid or 1-hydroxynaphthalene-2-carboxylic acid (5.30 mmol) and appropriate alkoxyaniline (5.30 mmol) were suspended in 30 mL of dry chlorobenzene. Phosphorous trichloride (2.65 mmol) was added dropwise, and reacting mixture was heated in the microwave reactor for 15 min at 130 C using infrared flask-surface control of temperature. Solvent was evaporated in vacuum; residue solid was washed with 2M HCl and crystallized from aqueous ethanol. If necessary, column chromatography was used for further purification (mobile phase DCM:MeOH 19:1).

The synthetic route of 7664-66-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Gonec, Tomas; Pospisilova, Sarka; Kauerova, Tereza; Kos, Jiri; Dohanosova, Jana; Oravec, Michal; Kollar, Peter; Coffey, Aidan; Liptaj, Tibor; Cizek, Alois; Jampilek, Josef; Molecules; vol. 21; 8; (2016);,
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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. 134364-69-5, name is 2,3-Difluoroanisole, A new synthetic method of this compound is introduced below., Recommanded Product: 2,3-Difluoroanisole

Example 1; 2′-Chloro-2,5-difluoro-4-methoxybenzophenone Aluminum chloride (92.54 g, 694 mmol) was transferred to a bottle (in a glove bag under dry N2), then to the reaction flask. Dichloromethane (600 mL) was added via syringe and the suspension cooled to 0 C. (ice-H2O bath). 2-Chlorobenzoyl chloride (88.2 mL, 121.45 g, 694 mmol) was added via syringe at 0-5 C. over 13 min. The addition funnel was rinsed with 10 mL dichloromethane. The difluoroanisole (77.8 mL, 100.0 g, 694 mmol) was then added dropwise via syringe at 0-5 C. over 13 min. The resulting yellow solution was stirred at 0-5 C. for 3.5 h (until the bath warmed) then at 20-25 C. for 14 h.The solution is poured over 600 g ice in a 2 L round bottom flask. Dichloromethane (80 mL) was used to complete the transfer. The layers were separated and the aqueous layer was extracted with 80 mL dichloromethane. The combined organic layers were transferred to a 1 L flask (with paddle stirrer) for distillation under dry N2. The dichloromethane is then replaced by n-heptane. At a bath temperature of 55-65 C., the head temperature is 35-38 C. and the pot temperature climbs to as high as 52 C. The pot solution is cooled and n-heptane (400 mL) is added. The distillation is continued. At a bath temperature of 100 C., the head temperature climbs from 55 to 75 C. and pot temperature climbs to as high as 83 C. before stopping the distillation (collected 767 mL total distillate). The pot suspension is now two phases, colorless on top and yellow on bottom. The suspension is allowed to cool to 50 C. and stirred at 200 rpm for 1 h. The suspension is allowed to cool to 40 C. and stirred at 200 rpm for 1 h. The suspension is allowed to cool to 30 C. and stirred at 200 rpm for 1 h. The 30 C. suspension is then cooled to 0-5 C. and stirred for 30 min. The precipitate is suction filtered (600 ml coarse sintered glass funnel), washed with 100 mL n-heptane at 0 C., and air dried 17 h at 25 C. to afford 181.23 g (92.4%) of light yellow solid.Recrystallization from hexanes provides colorless crystals, m.p. 84-85 C.; 500 MHz 1H NMR (CDCl3) delta 7.56 (dd, J=6.5 Hz, J=11.5 Hz, 1H), 7.43-7.39 (m, 3H), 7.38-7.34 (m, 1H), 6.65 (dd, J=6.6 Hz, J=11.5 Hz, 1H), 3.94 (s, 3H); 125 MHz 13C NMR (CDCl3) delta 190.2, 159.2 (dd, J=2 Hz, J=253 Hz), 153.9, 148.7 (dd, J=3 Hz, J=244 Hz), 140.0, 131.7, 131.21, 131.19, 130.2, 129.08, 129.07, 127.1, 117.5 (dd, J=3 Hz, J=21 Hz), 101.7 (dd, J=2 Hz, 29 Hz), 56.9; IR (KBr) 3057, 2986, 2941, 1663, 1653, 1620, 1519, 1443, 1420, 1360 cm-1. Elem. Anal. Calcd for C14H9ClF2O2: C, 59.49; H, 3.21; Cl, 12.54; F, 13.44. Found: C, 59.49; H, 3.13.

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; Roche Colorado Corporation; US2009/203901; (2009); A1;,
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Some common heterocyclic compound, 645-36-3, name is 2,2-Diethoxyethanamine, molecular formula is C6H15NO2, 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. Product Details of 645-36-3

2,2-Diethoxyethylamine (470 muL, 3.23 mmol) was added to a suspension of pyrimidine 9 (0.63 g, 2.67 mmol) in i-PrOH (30 mL), and the mixture was stirred at r.t. until the starting compound has dissolved. Et3N (560 muL, 4.0 mmol) was then added and the mixture was stirred for a further 45 min. H2O (50 mL) was added and the product was extracted with CH2Cl2 (2 × 50 mL). The organic layers were combined, washed with H2O (2 × 20 mL), dried (Na2SO4), and concentrated. The residue was purified by flash chromatography(silica gel, CH2Cl2; Rf = 0.42) to give a yellow solid; yield: 0.61 g(69%); mp 65.5-67.5 C.IR (KBr): 3380 (NH) cm-1. 1H NMR (300 MHz, CDCl3): delta = 1.27 (t, J = 6.9 Hz, 6 H, 2 × CH3),2.55 (s, 3 H, SCH3), 3.60 (dq, 2J = 9.3 Hz, 3J = 6.9 Hz, 2 H,2 × CHAHBCH3), 3.72-3.83 (m, 4 H, NCH2 and 2 × CHAHBCH3),4.09 (s, 3 H, OCH3), 4.68 (t, J = 5.4 Hz, 1 H, OCH), 8.84 (br s, 1 H,NH).13C NMR (75 MHz, CDCl3): delta = 14.8, 15.6, 44.3, 55.7, 63.2, 100.5,113.5, 156.6, 163.8, 174.6.Anal. Calcd for C12H20N4O5S: C, 43.36; H, 6.07. Found: C, 43.68;H, 6.11.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 645-36-3, its application will become more common.

Reference:
Article; Juskenas, Robertas; Masevicius, Viktoras; Tumkevicius, Sigitas; Synthesis; vol. 45; 17; (2013); p. 2438 – 2446;,
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Related Products of 41365-75-7,Some common heterocyclic compound, 41365-75-7, name is 1-Amino-3,3-diethoxypropane, molecular formula is C7H17NO2, 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.

Into a 25-mL round-bottom flask purged and maintained with an inert atmosphere of nitrogen, methyl (2S)-5-amino-6-bromo-2-methyl-1,2,3,4-tetrahydroquinoline-1-carboxylate (300 mg, 1.00mmol, Intermediate 1) was dissolved in toluene (5 mL). Then 3,3- diethoxypropan-1-amine (885 mg, 6.01mmol), 3rd Generation BrettPhos precatalyst (91 mg, 0.10mmol), BrettPhos (108 mg, 0.20mmol) and sodium tert-butoxide (289 mg, 3.01mmol) were added successively. The resulting solution was stirred for 2 h at 110oC under nitrogen atmosphere. The reaction mixture was cooled and the resulting solids were filtered out. The filtrate was concentrated under vacuum. The residue was subjected to purification by FCC eluting with ethyl acetate/petroleum ether (2:1). This afforded the title compound (240 mg, 62%) as a yellow oil. MS: (ES, m/z): 366 [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 1-Amino-3,3-diethoxypropane, its application will become more common.

Reference:
Patent; FORMA THERAPEUTICS, INC.; SCHILLER, Shawn E.R.; HERBERTZ, Torsten; LI, Hongbin; GRAVES, Bradford; MISCHKE, Steven; WEST, Angela V.; ERICSSON, Anna; DOWNING, Jennifer R.; (484 pag.)WO2019/55877; (2019); A1;,
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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. 93919-56-3, name is (4-(Trifluoromethoxy)phenyl)methanamine belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C8H8F3NO

General procedure: 5.3g (0.02 mol) of methyl N-nitro-1,3-dioxoisoindoline-2-carbimidothioate (3) was dissolved in 120 mL of acetonitrile, and cooled to 0-5, dropped in a quantity of 0.02 mmol of (aryl)methanamine over 5 mins. The reaction was stirred at 0-5 for one hour again. The mixture was filtered, concentrated in vacuo and recrystallised in EtOAc – petroleum ether (1:1) to give pure products 4a~4f.

The synthetic route of 93919-56-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wu, Qinglai; Zhao, Fenghai; Zhu, Xiang; Zhou, Ziyuan; Yang, Dongyan; Xu, Zhihong; Li, Junkai; Qin, Zhaohai; Natural Product Research; (2019);,
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Related Products of 929-75-9, A common heterocyclic compound, 929-75-9, name is 1,11-Diamino-3,6,9-trioxaundecane, molecular formula is C8H20N2O3, 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 for the preparation of compounds 10-15 (B) (0016) The appropriate diamines were added to compound 1a and Na2CO3 (2eq.) with stirring in DMF (5mL). The mixture was stirred overnight at room temperature. After completion, as judged by TLC, the solvent was evaporated under reduced pressure. The mixture was resolved in EtOAc and washed twice with water and brine. The organic layer was dried over Na2SO4, then filtered and concentrated. The crude product was purified by column chromatography (CH2Cl2/MeOH, 25/1 v/v) to give the target compound as a white solid.

The synthetic route of 929-75-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Yu, Fei; Peng, Yiyun; Wang, Qi; Shi, Yongying; Si, Longlong; Wang, Han; Zheng, Yongxiang; Lee, Emily; Xiao, Sulong; Yu, Maorong; Li, Yingbo; Zhang, Chuanling; Tang, Hengli; Wang, Chunguang; Zhang, Lihe; Zhou, Demin; European Journal of Medicinal Chemistry; vol. 77; (2014); p. 258 – 268;,
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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 592-55-2 as follows. Quality Control of 1-Bromo-2-ethoxyethane

To a solution of 3-(3-ethylazepan-3-yl)phenol (step a, 0.42 g, 1.92 mmol) in ACN (20 mL), N-ethyldiisipropylamine (0.67 mL, 3.830 mmcl) and 1-bromo-2-ethoxyethane (0.24 mL, 2.11 mmol) were added and the reaction mixture was heated at 65?C overnight. The reaction mixture was cooled and partitioned between 5% aqueous KHCO3 solution and AcOEt. The layers were separated and the organic layer wasdried over anh Na2SO4, filtered and concentrated to dryness. The crude product thus obtained was purified by flash chromatography on silica gel, gradient DCM/MeOH (0 to 10% MeOH) to give the title compound (0.15 g, 28% yield).HPLC-MS (Method A): Ret, 2.12 min; ESI-MS m/z, 292.4 (M+H).

According to the analysis of related databases, 592-55-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; LABORATORIOS DEL DR. ESTEVE, S.A.; MERCE-VIDAL, Ramon; ALMANSA-ROSALES, Carmen; GARCIA-LOPEZ, Monica; (148 pag.)WO2017/121645; (2017); A1;,
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Electric Literature of 41365-75-7,Some common heterocyclic compound, 41365-75-7, name is 1-Amino-3,3-diethoxypropane, molecular formula is C7H17NO2, 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 0.6 mmol of quinomethane 1a-1c and 0.6 mmol of 3,3-diethoxypropan-1-amine (2) or 4,4-diethoxybutan-1-amine (3) in 1 mL of 1,4-dioxane was stirred for 2-3 h at room temperature under argon. When the reaction was complete, the solvent was removed under reduced pressure (water-jet pump), and the residue was washed with hexane and dried in a vacuum (oil pump) until constant weight.

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

Reference:
Article; Vagapova; Amirova; Burilov; Pudovik; Sinyashin; Russian Journal of Organic Chemistry; vol. 51; 9; (2015); p. 1268 – 1271; Zh. Org. Khim.; vol. 51; 9; (2015); p. 1294 – 1297,4;,
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Reference of 494-99-5, 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. 494-99-5, name is 1,2-Dimethoxy-4-methylbenzene belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

(a) 80.0 g (0.6 mole) of aluminium chloride are introduced in portions, while stirring, into a solution of 84.1 g (0.5 mole) of 1,2-dimethoxy-4-methylbenzene (homopyrocatechol dimethyl ether or 4-methylveratrole) in 750 ml of 1,2-dichloroethane, during which the temperature is maintained at 20 maximum by cooling with an ice bath. Then, at 15-20, 85.0 g (approximately 73 ml, 0.55 mole) of phenyl acetyl chloride are added dropwise in the course of one hour, during which there is moderate evolution of hydrogen chloride and the aluminium chloride is dissolved. The reaction mixture is then stirred at room temperature for a further 6 hours and subsequently poured into 3000 ml of a mixture of ice and water. The resulting layers are separated and the organic phase is washed in succession with 2N hydrochloric acid, twice with water, then with 1N sodium bicarbonate solution and a further twice with water, dried, filtered and concentrated by evaporation. The partially crystallized residue is caused to crystallise completely from ether/petroleum ether (boiling range 40-65), 1-(4,5-dimethoxy-2-methylphenyl)-2-phenyl-1-ethanone having a melting point of 45-48 being obtained.

The synthetic route of 1,2-Dimethoxy-4-methylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Ciba-Geigy Corporation; US4500542; (1985); A;,
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