Tag: M.W=100-200

Some common heterocyclic compound, 22483-09-6, name is 2,2-Dimethoxyethanamine, molecular formula is C4H11NO2, 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: C4H11NO2

General procedure: A solution of amino acetaldehyde dimethyl acetal 2a (10. 514 g, 1.081 mL, 10 mmol), purchased from Alfa Aesa, and an aldehyde (10 mmol) in dry ethanol was placed in a round bottom flask and stirred for 12 h. To that solution, sodium borohydride powder (0.567 g, 15 mmol) was added at 0 C slowly over 5 minutes. the solution was then warmed to room temperature. After stirring for 4 h, the reaction was quenched with 3 drops of water and the mixture was filtered through a pad of celite. The solvent was evaporated under reduced pressure, the residue was extracted with 100 mL of ethyl ether and washed with100 mL of water. The organic layer was dried over MgSO4 anhydrous. Ethyl ether was then evaporated and the resulted viscous liquid was purified by flash column chromatography (SiO2; 4:1 then 3:1 and finally 1:1hexanes/ethyl acetate).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 22483-09-6, its application will become more common.

Synthetic Route of 1836-62-0,Some common heterocyclic compound, 1836-62-0, name is 2-(2-Methoxyphenoxy)ethylamine, molecular formula is C9H13NO2, 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: Compound 5a (100 mg, 0.42 mmol), and 2-(2-methoxyphenoxy)ethanamine (84 mg, 0.50 mmol) were added to ethanol and theresulting heterogeneous solution was reuxed for 24 h. Themixture was cooled to room temperature and ltered through a padof celite and the ltrate was concentrated under reduced pressure.The residue was puried by ash chromatography on silica-gelwith 10% methanol in ethyl acetate. Yielding 83% compound 9a(176 mg) as a white solid. Compound 9b was synthesized followingthe procedure of preparation 9a.

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

Reference of 349-55-3, The chemical industry reduces the impact on the environment during synthesis 349-55-3, name is 3-Methoxy-5-(trifluoromethyl)aniline, I believe this compound will play a more active role in future production and life.

3-methoxy-5- (trifluoromethyl)aniline (100 mg, 0.52 mmol) was dissolved in CHC13 (5.2 mL) and t-butyl nitrite (124 muL, 1.05 mmol) was added dropwise by syringe. Iodine (266 mg, 1.05 mmol) was added and then the reaction was slowly heated to 50C and was maintained at this temperature for an hour and thirty minutes. The reaction was then cooled to room temperature and poured into aq. NaHS03 (50 mL). The mixture was extracted with EtOAc (50 mL) and the organic extracts were washed with aq. NaHS03 (3 X 50 mL) and brine (20 mL), dried over Na2S04, filtered, and concentrated. Purification by flash chromatography with 1% to 15% EtOAc/hexanes afforded 1-iodo-3-methoxy-5-(trifluoromethyl)benzene. Rf= 0.75 (25% EtOAc/hexanes). ‘H NMR (CDC13, 500 MHz) 8 7.53 (s, 1H), 7.41 (s, 1H), 7.09 (s, 1H), 3.82 (s, 3H). Step B: 3-Methoxy-5-(trifluoromethyl)benzonitrile To a solution of 1-iodo-3-methoxy-5-(trifluoromethyl)benzene (200 mg, 0.66 mmol) in DMF (2 mL) was added CuCN (300 mg, 5.0 mmol). The reaction was stirred at 100C for 24 hours and then poured into aq. NH3 (40 mL). The mixture was extracted with EtOAc (70 mL) and the organic extracts were washed with brine (25 mL), dried over Na2S04, filtered, and concentrated. Purification by flash chromatography with 5% to 80% EtOAc/hexanes afforded 3-methoxy-5- (trifluoromethyl)benzonitrile. 0.64 (50% EtOAc/hexanes). ‘H NMR (CDC13, 600 MHz) 8 7.47 (s, 1H), 7.34 (s, 1H), 7.31 (s, 1H), 3.89 (s, 3H). Step C: 3-Methoxy-5-(trifluoromethyl)benzaldehyde A mixture of 3-methoxy-5- (trifluoromethyl)benzonitrile mg, 0.43 mmol) and Pt02 (9.8 mg, 0.043 mmol) in 88% formic acid (651 muL) was heated to 60C. The reaction was stirred at this temperature for thirty minutes. The reaction was then cooled to room temperature, diluted with hexanes (5 mL), loaded on a silica gel column, and purified with 1% to 15% EtOAc/hexanes to afford 3-methoxy-5- (trifluoromethyl) benzaldehyde. Rf= 0.56 (25% EtOAc/hexanes). ‘H NMR (CDCl3,500 MHz) 8 10.01 (s, 1H), 7.71 (s, 1H), 7.56 (s, 1H), 7.39 (s, 1H), 3.92 (s, 3H).

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, 3-Methoxy-5-(trifluoromethyl)aniline, other downstream synthetic routes, hurry up and to see.

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. 1116-77-4, name is 4,4-Diethoxy-N,N-dimethyl-1-butanamine, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 4,4-Diethoxy-N,N-dimethyl-1-butanamine

Sodium nitrite (16 gm) in water (120 ml) was added slowly for a period of 30 minutes at 0 deg C to a solution of (S)-4-(4-Aminobenzyl)-2-oxazolidinone (40 gm), concentrated hydrochloric acid (46 ml) and water (480 ml) in round bottomed flask, cooled to 0 deg C and stirred for 1 hour. The above diazotized solution was added for a period of 30 minutes at 0 deg C to sodium sulfite (78.3 gm) in water (200 ml) in another round bottomed flask, cooled to 0 deg C, slowly allowed to room temperature, heated to 55 deg C and stirred for 15 minutes at 60 deg C. Added concentrated hydrochloric acid (80 ml) to the reaction mass, stirred for 16 hours at 60 deg C, nitrogen gas was applied and heated to 90 deg C. Water (80 ml) was added to the reaction mass for 15 minutes at 90 deg C, added 4-(dimethylamino)-butyraldehyde diethylacetal for a period of 40 minutes, heated to reflux, stirred for 3 hours at reflux, cooled to 25 – 30 deg C and the pH was adjusted to 7 by adding sodium hydroxide solution(30%, 230 ml). Extracted with ethyl acetate (7 X 200 ml), adjusted the pH of the aqueous layer to 10 by adding sodium hydroxide solution (30%, 100 ml), heated to 50 deg C and again extracted with ethyl acetate (8 X 200 ml) at 50 deg C. Both the organic layers were combined, dried with sodium sulfate, given carbon treatment and the solvent was distilled off completely under vacuum at 50 – 55 deg C, ethyl acetate (80 ml) was added to the reaction mass at 25 deg C, stirred for 1 hour and cooled to 10 deg C. Stirred for 30 minutes at 10 deg C, filtered the material and washed with chilled ethylacetate(20 ml) under nitrogen atmosphere and dried at 45 -50 deg C to yield 40 gm of (4S)-4-[[3-[2-(Dimethylamino)ethyl]~ 1 H-indol-5-yl]methyl]-2-oxazolidinone.(4S)-4-[[3-[2-(Dimethylamino)ethyl]-1H-indol-5-yl]methyl]-2-oxazolidinone (40 gm, Zolmitriptan) was dissolved in isopropanol (200 ml) at 25 deg C, heated to reflux, stirred for 40 minutes at reflux and slowly allowed to cool to 0 deg C. Stirred the reaction mass for 1 hour at 0 deg C, filtered the compound, washed with chilled isopropanol(40 ml) and dried at 40 – 45 deg C under vacuum to yield (4S)-4-[[3-[2-(Dimethylamino)ethyl]-1H-indol-5-yl]methyl]-2-oxazolidinone isopropanol solvate (32 gm, Zolmitriptan isopropanol solvate; HPLC purity. 99.32%). Zolmitriptan isopropanol solvate obtained above (32 gm) was dissolved in isopropyl acetate (2250 ml) at 25 deg C. Then the contents were heated to reflux and maintained for 30 minutes to form clear solution. The solution was cooled to 25 deg C during a period of 1 hour. The separated solid was filtered, washed with isopropyl acetate (160 ml) to obtain 32 gm of zolmitriptan isopropyl acetate solvate (HPLC purity: 99.8%).

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 1116-77-4.

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. 19500-02-8, name is 3-Methoxy-2-methylaniline, A new synthetic method of this compound is introduced below., Safety of 3-Methoxy-2-methylaniline

The 15.0g of 3-amino-1-methoxy-2-methylbenzene mixture, 48.7g of triphosgene and 350ml of toluene was heated under reflux for 3 hours with stirring. The reaction mixture was allowed to cool and concentrated under reduced pressure to give 17.0g of 1-methoxy-3-isocyanato-2-methylbenzene.

The synthetic route of 19500-02-8 has been constantly updated, and we look forward to future research findings.

Reference of 1535-73-5, The chemical industry reduces the impact on the environment during synthesis 1535-73-5, name is 3-Trifluoromethoxyaniline, I believe this compound will play a more active role in future production and life.

General procedure: To the stirred mixture of benzaldehyde (0.20 mL, 2.0 mmol) and amine (2.0 mmol, aniline: 0.18 mL, 4-toluidine: 0.21 g, biphenyl-4-amine: 0.34 g, 4-fluoroaniline: 0.19 mL, 4-chloroaniline: 0.26 g, 4-bromoaniline: 0.24 g, 4-nitroaniline: 0.28 g, ethyl 4-aminobenzoate: 0.33 g, 4-methoxyaniline: 0.25 g, 3,4-dimethoxyaniline: 0.31 g, 2-(methylthio)aniline: 0.25 mL, 2-aminobenzophenone: 0.39 g, 3-phenoxyaniline: 0.37 g, 3-(trifluoromethyl)aniline: 0.25 mL, 3-(trifluoromethoxy)aniline: 0.27 mL, naphthalene-1-amine: 0.29 g) was added (1.2 mL, 2.0 mmol) of T3P (Aldrich 50percent solution in EtOAc). If the mixture did not become a solution, (in the cases of the examples covered by entries 3 and 7 of Table 1) CH2Cl2 (2 mL) and EtOAc (2 mL) were added. After 5 min, (0.35 mL, 2.0 mmol) of P(OEt)3 was added and the mixture was stirred at 26 °C. After completion of the reaction (5?10 min), the mixture was diluted with EtOAc (15 mL) and washed with 10percent NaHCO3 solution (15 mL). The organic phase was dried (Na2SO4), filtered and concentrated. The residue was purified by flash chromatography on silica gel (Merck 107736 Silica gel 60H, CH2Cl2?MeOH) to afford products 3a?p.

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, 3-Trifluoromethoxyaniline, other downstream synthetic routes, hurry up and to see.

102-52-3, name is 1,1,3,3-Tetramethoxypropane, belongs to ethers-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. SDS of cas: 102-52-3

Example 1: Ethyl fl2-Amino-3-chloro-6,7,10,ll-tetrahydro-7,ll- methanocycloocta[61 quinolin-9-yl)acetate (HUP 1)Preparation of tetramethyl 3,7-Dihydroxybicyclo[3.3.11nona-2,6-diene-2,4,6,8- tetracarboxylateA mixture of 1,1,3,3 tetramethoxypropane (32.8 g, 0.20 mol) and 2 M HC1(100 mL) was stirred for 1.5 h at room temperature. To this mixture cooled at 0C was added successively and carefully an aqueous solution of 5 M NaOH within 30 min (pH = 8) and MeOH (100 mL). At 0C, dimethyl-3-oxoglutarate (69.6 g, 0.40 mol) was added, followed by addition of MeOH (70 mL). The reaction mixture was allowed to warm to room temperature and stirred for 3 days. The reaction mixture was acidified to pH = 3 with 10 M HC1. Filtrating fractionwise, washing with water and drying at the dessicator afford the desired tetra ester as a white solid (39.2 g, 51%).

The synthetic route of 102-52-3 has been constantly updated, and we look forward to future research findings.

Electric Literature of 7252-83-7,Some common heterocyclic compound, 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane, molecular formula is C4H9BrO2, 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 round bottom flask was added 4-(morpholinyl)thiobenzamide (2.22 g, 10 mmol) and dissolved in ethanol (50 mL).Then 2-bromo-1,1-dimethoxyethane (1.69 g, 10 mmol) and p-toluenesulfonic acid (1.90 g, 10 mmol) were added while stirring, and the reaction system was heated to 95C and reacted overnight.After the reaction was completed, the mixture was cooled to room temperature and filtered to give a solid which after drying gave a yellow solid (2.00 g, 81%).

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

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. 4393-09-3, name is (2,3-Dimethoxyphenyl)methanamine, A new synthetic method of this compound is introduced below., Product Details of 4393-09-3

EXAMPLE 13 2-[Trans-(4-aminocyclohexyl)amino]-6-[(2,3-dimethoxybenzyl)amino]-9-cyclopentylpurine dihydrochloride Scheme A, step b: 2-Chloro-6-[(2,3-dimethoxybenzyl)amino]-9-cyclopentylpurine 2-Chloro-6-[(2,3-dimethoxybenzyl)amino]-9-cyclopentylpurine is prepared from 2,6-dichloro-9-cyclopentylpurine, 2,3-dimethoxybenzylamine, and triethylamine essentially as described above in Example 1, Scheme A, step b. Scheme A, step c: 2-[Trans-(4-aminocyclohexyl)amino]-6-[(2,3-dimethoxybenzyl)amino]-9-cyclopentylpurine dihydrochloride 2-[Trans-(4-aminocyclohexyl)amino]-6-[(2,3-dimethoxybenzyl)amino]-9-cyclopentylpurine dihydrochloride is prepared from 2-chloro-6-[(2,3-dimethoxybenzyl)amino]-9-cyclopentylpurine essentially as described in Example 1, Scheme A, step c.

The synthetic route of 4393-09-3 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 701-56-4, name is 4-Methoxy-N,N-dimethylaniline, 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 701-56-4, category: ethers-buliding-blocks

General procedure: A round-bottom flask was chargedwith N,N-dialkyl aniline dissolved in toluene solution, under N2 condition. TBHP was added drop wise and reaction was stirred for 2 min. Triethylamine was added thereafter, and then the contents of the reaction were stirred for 3 h at 110 C under inert N2 condition. The reaction mixture was washed 2-3 times with H2O and ethyl acetate. The upper organic layer was separated and dried over sodium sulphate and then subjected to rotavapour. The crude mixture was purified by column chromatography on silica gel (60-120).

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