Month: April 2021

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. 450-88-4, name is 1-Bromo-4-fluoro-2-methoxybenzene, A new synthetic method of this compound is introduced below., Safety of 1-Bromo-4-fluoro-2-methoxybenzene

A mixture of 1 -bromo-4-fluoro-2-methoxybenzene (CAS No. [450-88-4]; 10.0 g, 48.8 mmol) in concentrated sulfuric acid (50 mL) was cooled to 0 C and treated dropwise with a freshly prepared mixture of fuming nitric acid (1.05 eq., 2.1 mL, 51 mmol) and concentrated sulfuric acid (1.85 eq., 4.8 mL, 90 mmol). The reaction mixture was stirred at 0 C for 30 minutes and poured in small portions on ice water. The formed precipitate was filtered off, washed with cold water and kept. The filtrate was extracted with ethyl acetate and the organic layer combined with the isolated precipitation. The organic layer was dried with sodium sulfate and concentrated in vacuo. The obtained material was purified by flash chromatography (SiO2-hexane/ ethyl acetate) to give the title compound (5.88 g, 44%). (0555) 1H-NMR (400MHz, DMSO-d6): [ppm] = 4.00 (s, 3H), 7.44 (d, 1 H), 8.40 (d, 1 H).UPLC- MS (ESI-): [M – H]- = 248/250; Rt = 1.17 min (Br isotope pattern; Method E).

The synthetic route of 450-88-4 has been constantly updated, and we look forward to future research findings.

Electric Literature of 102-52-3, A common heterocyclic compound, 102-52-3, name is 1,1,3,3-Tetramethoxypropane, molecular formula is C7H16O4, 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.

To a suspension of intermediate lId (1.834 g, 8.94 mmol) in EtOH (30 ml) were added malonaldehyde bis(dimethyl acetal) (1.63 ml, 9.84 mmol) and conc.HC1 (1 ml). The reaction mixture was stilTed at 70C for 2 hours. The cooled mixture was evaporated todryness, diluted saturated solution of NaHCO3 and extracted with EtOAc twice. The combined organics were washed with water, with saturated solution of NaC1, dried over MgSO4, filtered and evaporated. The final product was purified by silica gel chromatography using 0 to 30 % EtOAc/cyclohexane as eluent to give intermediate lie(1.380 g, 64%). ?H NMR (500 MHz, CDC13) oe 8.12 (d, J= 2.1 Hz, 1H), 7.94 (s, 1H), 7.85 (d, J= 8.3 Hz, 1H), 7.72 (d, J= 1.4 Hz, 1H), 7.40 (s, 1H), 7.36 (dd, J= 8.3, 1.8 Hz, 1H),7.32 (d, J= 1.7 Hz, 1H), 6.46-6.43 (m, 1H), 3.97 (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.

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. Recommanded Product: 1-Bromo-2-ethoxyethane

In a similar manner 1d was obtained from sodium (diglyme)2 3,4,5-triphenyl-1,2-diphosphacyclopentadienide (0.94 g, 1.52 mmol) and 1-bromo-2-ethoxyethane BrCH2CH2OEt (0.26 g, 1.90 mmol, 25% excess) as a light-yellow oil; yield 0.36 g (59%). 1H NMR (CDCl3): 0.59 (t, 3H, 3JHH = 6.9, 3), 1.42-1.47 (m, 2H, OCH2), 1.51-1.57 (m, 2H, OCH2), 1.88-1.93 (m, 2H, PCH2), 6.85 (d, 4H, 3JHH = 3.42), 6.90 (d, 2H, 3JHH = 7.34), 6.96 (d, 4H, 3JHH = 6.85), 6.99-7.07 (m, 1H, 3JHH = 5.38), 7.20 (d, 2H, 3JHH = 7.34), 7.29 (d, 2H, 3JHH = 5.87). 31P NMR (CDCl3): 51.9 (d, 1JPP = 407.3), 214.1 (d, 1JPP = 407.3). 13 NMR (CDCl3): 16.7 (s, CH3), 25.6 (s, CH2), 27.3 (d, 2JCP = 9.7, CH2), 37.8 (dd, 1JCP = 16.3, 2JCP = 5.8, CH2), 126.4 (s, p-Ph), 126.5 (s, p-Ph), 126.8 (s, p-Ph), 127.4 (s, m-Ph), 128.2 (s, m-Ph), 128.3 (s, m-Ph), 128.5 (s, o-Ph), 129.2 (s, o-Ph), 130.5 (d, 3JCP = 1.4, o-Ph), 131.7 (s, o-Ph), 133.5 (s, o-Ph), 137.6 (d, 3JCP = 6.2, ipso-Ph), 138.24 (dd, 3JCP = 10.4, 3JCP = 3.8, ipso-Ph), 142.8 (d, 3JCP = 9.8, ipso-Ph), 149.7 (ps.tr, 3JCP = 15.51, C4), 164.5 (dd, 1JCP = 7.3, 2JCP = 3.1, C5), 185.8 (dd, 1JCP = 47.1, 2JCP = 14.9, C3).

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.

Related Products of 75148-49-1,Some common heterocyclic compound, 75148-49-1, name is 3-Bromobenzaldehyde Diethyl Acetal, molecular formula is C11H15BrO2, 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.

7c) In analogy to Example 7a), from 1-bromo-3-diethoxymethyl-benzene (Example 6c)) and ethyl 1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-7-[[(trifluoromethyl)sulphonyl]oxy]-quinoline-3-carboxylate there is obtained ethyl 1-cyclopropyl-7-(3-diethoxymethyl-phenyl)-6-fluoro-1,4-dihydro-4-oxo-quinoline-3-carboxylate as a colourless solid. Yield: 44%. Mass spectrum: peaks: inter alia at 453 (M+, 16%), 408 (21%), 381 (100%).

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

Adding a certain compound to certain chemical reactions, such as: 62415-74-1, name is 1,2-Dibromo-4-methoxybenzene, 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 62415-74-1, name: 1,2-Dibromo-4-methoxybenzene

The zinc reagent 2b was prepared according to TP1 from 1,2-dibromo-4-methoxybenzene (1b, 3.98 g, 15 mmol), Zn-powder(2.94 mg, 45 mmol) and InCl3 (0.25 g, 1.13 mmol). The reaction was carried out in 15 mL DMPU at 50 C for 2 h. Iodolysis indicated a yield of 59% bimetallic reagent (8.85 mmol). The solution containing the zinc reagent was separated from the remaining zinc powder and transferred to a new flask containing a solution of methyl 4-iodobenzoate (3k, 788 g,30 mmol) and PEPPSI-iPr (0.14 g, 0.21 mmol) in THF (15 mL).The reaction mixture was stirred at 50 C for 12 h before being quenched with HCl (2 M, 40 mL). Flash column chromatographical purification on silica gel (pentane/diethylether = 5:1) afforded 4m as a white solid (2.37 g, 6.29 mmol,71%).

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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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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.

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. 4698-11-7, name is 10-Methoxy-5H-dibenzo[b,f]azepine, A new synthetic method of this compound is introduced below., name: 10-Methoxy-5H-dibenzo[b,f]azepine

Following the procedure of Example 4, but using dichloromethane as the solvent instead of toluene, at the reflux temperature, the yield is 52.0 (68.7% on theoretical).

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.

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.

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.