Tag: M.W=100-200

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. 64465-53-8, name is 4-Fluoro-3-methoxyaniline, A new synthetic method of this compound is introduced below., Quality Control of 4-Fluoro-3-methoxyaniline

Dissolve 4-fluoro-3-methoxyphenylamine (5. 0 g, 35 mmol) in water (25 mL) and concentrated sulfuric acid (8 mL). Cool to less than 0 C in an ice/methanol bath and add sodium nitrite (2. 7 g, 39 mmol) dropwise in a solution in water (20 mL) and stir one h. Dissolve potassium iodide (9. 9 g, 60 mmol) in water (35 mL) and add dropwise. Warm to room temperature and stir 18 h. Extract with ethyl acetate (300 mL), wash with water (200 mL), saturated aqueous sodium thiosulfate (300 mL), and saturated aqueous sodium chloride (300 mL). Dry (sodium sulfate), filter, and concentrate to give the title compound as an orange oil (8. 8 g, 99%). H NMR (300 MHz, CDCl3) 6 3. 88 (s, 3H), 6. 77-6. 87 (m, 1H), 7. 16-7. 26 (m, 2H).

The synthetic route of 64465-53-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ELI LILLY AND COMPANY; WO2005/94822; (2005); A1;,
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Electric Literature of 645-36-3, These common heterocyclic compound, 645-36-3, name is 2,2-Diethoxyethanamine, 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.

Compound 3 was prepared by the condensation of commercially available aminoacetaldehyde diethyl acetal with the phthalic anhydride (1:1 mol ratio), using toluene under reflux, in the presence of a catalytic amount of DMAP (yield 52%) for 2 h. In the next step, 2-(2,2-diethoxyethyl)isoindoline-1,3-dione (3) underwent acid hydrolysis (sulphuric acid at 70%) in reflux for 2 h. After the reaction was completed, it was allowed to reach at room temperature and was then cooled to induce precipitation. The formed precipitate was filtered on a sintered funnel with distilled water, yielding 55% of the pure product. For the synthesis of 5a and 5b, 2-(1,3-dioxoisoindol-2-yl) acetaldehyde (4) reacted with thiosemicarbazide (in the ratio 1:1) (for 5a) or 4-phenyl-3-thiosemicarbazide (for 5b), in ethanol, under reflux with catalytic amount of HCl (4 drops) for 4 h. The reactions were followed by thin layer chromatographic plate analysis. The formed precipitate was filtered on a sintered funnel with ethanol to yield the pure product (yield 76% for 5a and 70% for 5b).

Statistics shows that 2,2-Diethoxyethanamine is playing an increasingly important role. we look forward to future research findings about 645-36-3.

Reference:
Article; De Moraes Gomes, Paulo Andre Teixeira; Oliveira, Arsenio Rodrigues; De Oliveira Cardoso, Marcos Verissimo; De Farias Santiago, Edna; De Oliveira Barbosa, Miria; De Siqueira, Lucianna Rabelo Pessoa; Moreira, Diogo Rodrigo Magalhaes; Bastos, Tanira Matutino; Brayner, Fabio Andre; Soares, Milena Botelho Pereira; De Oliveira Mendes, Andresa Pereira; De Castro, Maria Carolina Accioly Brelaz; Pereira, Valeria Rego Alves; Leite, Ana Cristina Lima; European Journal of Medicinal Chemistry; vol. 111; (2016); p. 46 – 57;,
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Application of 7252-83-7, A common heterocyclic compound, 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane, molecular formula is C4H9BrO2, 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.

Following a modified procedure,[9] under a N2 atmosphere, 8a (867 mg, 1.44 mmol) andCs2CO3 (3.05 g, 9.36 mmol) were placed in a 100 mL sealed tube. 2-Bromo-1,1-dimethoxyethane (9) (1.60 g, 9.5 mmol) and solvent DMF (30 mL) were added via cannula.The reaction mixture was stirred at 110 C for 24 h. At ambient temperature, the mixture wasdiluted with EtOAc (250 mL) and washed with H2O (3¡Á60 mL) and brine (60 mL). Theorganic phase was dried over Na2SO4 and concentrated. The residue was purified by columnchromatography over silica gel (n-hexane/EtOAc 5/1) to give S10 (804 mg, 81%) as acolorless solid. M. p. = 162-163 C. 1H NMR (300 MHz, CDCl3) delta = 6.92 (s, 1H), 6.91 (s,1H), 6.92-6.78 (m, 4H), 6.79 (d, J = 8.8 Hz, 1H), 6.71 (d, J = 1.1 Hz, 1H), 4.85 (t, J = 5.5 Hz1H), 4.62-4.41 (m, 5H), 3.65 (s, 3H), 3.63 (s, 3H), 3.45 (s, 3H), 3.31 (s, 6H), 1.38 (d, J =6.1 Hz, 6H), 1.33 (d, J = 6.1 Hz, 6H), 1.31 (d, J = 6.1 Hz, 6H). 13C NMR (125 MHz, CDCl3)delta = 155.6 (Cq), 150.1 (Cq), 149.5 (Cq), 147.4 (Cq), 147.2 (Cq), 146.5 (Cq), 146.2 (Cq), 146.1(Cq), 144.0 (Cq), 127.7 (Cq), 127.4 (Cq), 123.8 (CH), 123.4 (CH), 122.2 (Cq), 118.5 (Cq),115.9 (CH), 115.2 (CH), 115.0 (CH), 114.6 (Cq), 114.5 (CH), 110.2 (Cq), 105.3 (CH), 104.4(CH), 103.5 (CH), 71.5 (CH), 71.5 (CH), 71.2 (CH), 55.9 (CH3), 55.8 (CH3), 55.6 (CH3), 55.3(CH3), 47.9 (CH2), 22.1 (CH3), 21.9 (CH3). IR (neat): 2975, 2931, 1703, 1517, 1463, 1257,1107, 1031, 752 cm-1. MS (ESI) m/z (relative intensity) 712 (100) [M+Na+], 690 (50)[M+H +], 658 (80). HR-MS (ESI) m/z calcd for C39H48NO10 [M+H+] 690.3273, found690.3267.

The synthetic route of 7252-83-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Mei, Ruhuai; Zhang, Shou-Kun; Ackermann, Lutz; Synlett; vol. 28; 14; (2017); p. 1715 – 1718;,
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Electric Literature of 145903-31-7, 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. 145903-31-7, name is 7-Methoxy-2,3,4,5-tetrahydrobenzo[f][1,4]thiazepine belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Step 2: To a stirred solution of 2-(benzyloxy)ethanol (17.0 g, 1 1 1 .84 mmol) and PPh3 (35.0 g, 134.21 mmol) in DCM (170 mL) at -10 Patent; GRUeNENTHAL GMBH; FRANK, Robert; CHRISTOPH, Thomas; SCHIENE, Klaus; DE VRY, Jean; DAMANN, Nils; LESCH, Bernhard; BAHRENBERG, Gregor; SAUNDERS, Derek John; STOCKHAUSEN, Hannelore; KIM, Yong-Soo; KIM, Myeong-Seop; LEE, Jeewoo; WO2013/68461; (2013); 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. 1579-40-4, name is Di-p-tolyl Ether belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: Di-p-tolyl Ether

Representative Experimental Protocol: 2,7-Dimethyl-9-(4-nitro)phenyl xanthen-9-ol (R = NO2: 3e): Di-p-tolyl ether (1, 5 g, 25.5 mmol), 4-nitro benzoic acid (5.13 g, 30.7 mmol) and ZnCl2 (10 g, 73.4 mmol) are taken into a 100 ml double neck RB flask and charged with POCl3 (7.5 mL) and heated to 95 C for 4 h. The reaction mixture turned into a brown viscous mass that was difficult to stir. The reaction mixture was then cooled to room temperature and crushed ice was added slowly while keeping the low temperature. To the above mixture was added H2O (75 mL) and stirred for 12 h. The above reaction mixture was filtered and the residue was washed with H2O (20 mL) and hexane (20 mL) to afford 4-nitro-DMPx 3e as white powder. The crude product was dissolved in EtOAc and washed with NaHCO3 to remove the excess of 4-nitro benzoic acid. The EtOAc layer was evaporated under reduced pressure to furnish the desired product as fine powder 7.5 g (86%).

The synthetic route of 1579-40-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Banerjee, Shyamapada; Srishylam; Rajendra Prasad; Migawa, Michael T.; Swayze, Eric E.; Sanghvi, Yogesh S.; Tetrahedron Letters; vol. 53; 35; (2012); p. 4669 – 4672;,
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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. 10541-78-3, name is 2-Methoxy-N-methylaniline belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 10541-78-3

Bromoacetyl chloride (0.425 mL, 5.1 mmol) in dry dichloromethane (5 mL) was added dropwise to a solution containing the respective amine (4.1 mmol) and a catalytic amount of dimethylaminopyridine (DMAP) (0.150 g, 30 mmol %) in dry dichloromethane (20 mL) maintained in an ice bath under argon atmosphere. The resulting solution was stirred at 0 C for 30 min, and the temperature was then increased to 25 C. After stirring for additional 4 hours, the reaction mixture was diluted with diethyl ether (50 mL). All of the stirring time was accomplished under an argon atmosphere. The organic layers were washed sequentially with a solution of 1 N HCl (2 ¡Á 50 mL), water (1 ¡Á 100 mL), saturated aqueous NaHCO3 (3 ¡Á 50 mL), and brine (5% w/v, 1 ¡Á 50 mL). Finally, the organic solution was dried over anhydrous MgSO4 and evaporated under vacuum, and the residue was purified by flash chromatography on silica gel and eluted with chloroform-methanol (40:1).

The synthetic route of 10541-78-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Giacobbo, Bruno Couto; Pissinate, Kenia; Rodrigues-Junior, Valnes; Villela, Anne Drumond; Grams, Estevao Silveira; Abbadi, Bruno Lopes; Subtil, Fernanda Teixeira; Sperotto, Nathalia; Trindade, Rogerio Valim; Back, Davi Fernando; Campos, Maria Martha; Basso, Luiz Augusto; Machado, Pablo; Santos, Diogenes Santiago; European Journal of Medicinal Chemistry; vol. 126; (2017); p. 491 – 501;,
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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. 20781-20-8, name is (2,4-Dimethoxyphenyl)methanamine, A new synthetic method of this compound is introduced below., Quality Control of (2,4-Dimethoxyphenyl)methanamine

Added to the Schlenk reaction tube 18.1 mg (0.10 mmol) copper acetate, 16.0 mg (0.025 mmol) three (2, 2′ – bipyridyl) ruthenous, 16.0 mg (0.02 mmol) tert lithium ethoxide, using Schlenk double-row tube vacuum pumping, access oxygen state, adding 79 uL (0.5 mmol) 2, 4 – dimethoxybenzylamine, 2.5 ml dimethyl sulfoxide, the use of the Schlenk tube with double row sustained and the oxygen to the reaction system, the temperature control of the reaction system 35 C, white light LED lamp (wavelength 400 – 760 nm) irradiation, stirring for 20 hours after the, adding 3 ml saturated sodium acid sulfite aqueous solution and 10 ml ethyl acetate, extraction liquid, anhydrous magnesium sulfate drying, to remove the magnesium sulfate, the resulting organic phase is concentrated, the concentrate with silica gel column chromatography, to obtain 2, 4 – dimethoxy carbonitrile, yield 90%

The synthetic route of 20781-20-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; HUAIHAI INSTITUTE OF TECH; Huaihai Technology College; TAO CHUANZHOU; Tao Chuanzhou; WANG BIN; Wang Bin; SUN LEI; Sun Lei; LIU ZHOU; Liu Zhou; ZHAI YADONG; Zhai Yadong; (5 pag.)CN107814751; (2018); A;,
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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. 34967-24-3, name is 3,5-Dimethoxybenzyl amine, A new synthetic method of this compound is introduced below., Formula: C9H13NO2

In a procedure analogous to Example 21, reaction of 3, 5-dimethoxybenzylamine and 2, [6-DICHIOROPYRAZINE FURNISHED THE PRODUCT (91%).] 1H-n. [M.] [R.] (CDCl3) [No.3. ]78 [(S,] 6H, OCH3), 4.49 (d, J= 5.4 Hz, [2H,] NCH2); 5. 12 (br [S,] [1H,] NH), [6.] 39 [(T,] J= 2. 1 Hz, 1H, ArH), 6.50 (d, J= 2.1 Hz, 2H, ArH), 7.75 (s, 1H, pyraz.- H), 7. [S2] [(S,] 1H pyraz.-H).

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; CYTOPIA PTY LTD; WO2003/99796; (2003); A1;,
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Application of 1579-40-4, The chemical industry reduces the impact on the environment during synthesis 1579-40-4, name is Di-p-tolyl Ether, I believe this compound will play a more active role in future production and life.

Tolyl Ether (5.9 gm, 30 mmoles), bipheylcarboxylic acid (6 gm, 30.27 mmoles), zinc chloride (12 gm, 88 mmoles) and phosphorus oxychloride (20 mmoles) were stirred at 95 degree in an oil bath for 2 hrs. The mixture was cooled to room temperature and the viscous mixture is poured into cracked ice and stirred overnight. The solid was collected and washed with water. The solid was suspended in 150 ml of methanol and was heated to boiling for 5 min. The mixture was cooled to room temperature, filtered and dried to a constant weight (8.4 g, yield: 74%).

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, Di-p-tolyl Ether, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ISIS PHARMACEUTICALS, INC.; WO2005/77966; (2005); A1;,
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Adding a certain compound to certain chemical reactions, such as: 10541-78-3, name is 2-Methoxy-N-methylaniline, belongs to ethers-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 10541-78-3, Quality Control of 2-Methoxy-N-methylaniline

This compound was obtained by reacting 2-methoxy-N-methylaniline (3.0 g, 21.9 mmol.) and cyclopentanone (9.20 g, 109mmol) in the presence of a catalytic amount of iodine (278 mg, 1.09 mmol).After purification on a silica gel column using hexanes-ethyl acetate (95: 5),compound 10a was obtained as a yellowish oil (2.35 g, 42%). 1H NMR (CDCl3, 400 MHz): delta 1.68-1.72(2H, m), 1.76-1.82 (2H, m), 1.85-1.92 (2H, m), 2.01-2.07 (2H, m), 2.51-2.56(2H, m),2.65-2.70 (2H, m), 4.05 (3H, s), 4.47 (1H, brs, NH), 5.01 (1H, m), 6.03(1H, m), 6.58 (1H, d, J = 7.6 Hz),6.60 (1H, d, J = 4.0 Hz), 6.65 (1H,dd, J = 7.6 and 4.0 Hz). 13CNMR (CDCl3, 100 MHz): delta 22.6, 24.1, 31.6, 32.4, 40.2, 55.8, 64.8,109.3, 115.9, 116.3, 120.5, 132.2, 132.3, 138.8, 145.4. EI-MS (GC-MS): m/z(5) 255 [M]+ (30), 227(100), 213(15)

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-Methoxy-N-methylaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Fotie, Jean; Ayer, Suraj K.; Poudel, Binit S.; Reid, Carolyn S.; Tetrahedron Letters; vol. 54; 51; (2013); p. 7069 – 7073;,
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