Month: April 2021

Electric Literature of 82998-57-0, 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. 82998-57-0, name is 3-Iodo-4-methylbenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of 3-iodo-4-methylbenzoic acid (628 mg, 2.2mmol) in SOCl2 (20 mL) was added two drops of DMF. After heatingunder reflux for 2 h, the SOCl2 was evacuated, and the residue was dissolved in anhydrous THF (6 mL) to form light yellow solution.

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

Related Products of 672-57-1, 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 672-57-1 as follows.

12336] Three point eight (3.8) ml of n-butyllithium (2.6 M hexane solution) was added dropwise to a mixture of 3.00 g of 1 -chloro-2-iodo-4-(trifluoromethyl)benzene and 15 ml oftetrahydrofuran at -70 C., followed by stirring for 30 minutes. Thereafier, a mixture of 1.69 g of N-methoxy-N-methyltrifluoroacetamide and 5 ml of tetrahydrofuran was added drop- wise thereto at -70 C. Subsequently, afier the reaction mixture was stirred for 1 hour at room temperature, water was added thereto, and extraction was performed using ethyl acetate. The organic layer was washed with saturated saline, dried over magnesium sulfate, and then concentrated under reduced pressure. The residues were subjected to silica gel column chromatography, thereby obtaining 1.66 g of 2,2,2- trifluoro-1 -[2-chloro-5-(trifluoromethyl)phenyl]ethanone.

According to the analysis of related databases, 672-57-1, the application of this compound in the production field has become more and more popular.

Related Products of 52548-14-8,Some common heterocyclic compound, 52548-14-8, name is 2-Iodo-5-methylbenzoic acid, molecular formula is C8H7IO2, 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.

EXAMPLE EMethyl 2-iodo-5-methylbenzoate (E-I) A visually clean 100 L flask equipped with a mechanical stirrer thermocouple and water chilled condenser was charged with MeOH (50 L). 2-iodo-5-methylbenzoic acid (5.85 kg, 22.32 mol) was then added while stirring. Concentrated sulfuric acid (0.595 L, 11.16 mol) was then added portion- wise which caused an increase in temperature from 17 0C to 22 0C. This mixture was gradually brought to an internal temperature of 64.6 0C an aged overnight (~18h). The next morning the reaction had reached >98% conversion by HPLC. The flask was cooled to 160C by placing in an ice bath and 850ml of ION NaOH (0.98 equiv.) was added slowly (over 10 minutes) while monitoring the pH. After the addition the pH was 5-6 (Caution: bringing pH over 9 can result in saponification during the work-up). The solution was then concentrated to about 16L and this suspension was transferred to a 100 L extractor. The flask was rinsed with 8L of IPAc and 4L of water which were also transferred to the extractor. 32L IPAc along with 1OL of 5w% NaHCO3 and ~10L of 15w% Brine. The layers were cut and the aqueous layers were back- extracted with 2OL of IPAc. The organic layers were then combined and washed with 1OL of 15w% Brine. The organic layers were collected to provide E-I (6.055 kg, 21.93 mol, 98 % yield) in 98.3% purity.

The synthetic route of 52548-14-8 has been constantly updated, and we look forward to future research findings.

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. 452-79-9, name is 2-Fluoro-1-iodo-4-methylbenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C7H6FI

25mL reaction flask, adding 360mg (5.6mmol) copper powder, vacuuming for three times, then injecting 10mL dimethyl sulfoxide, 472mg (2mmol) 4-methyl-2-fluoroiodobenzene, 609mg (3mmol) ethyl bromodifluoroacetate, reacted at 80C overnight, the next day, the temperature was lowered to room temperature, extracted with 50 mL of ethyl acetate, washed with saturated sodium chloride solution, dried over anhydrous sodium sulfate, the solvent was distilled off by rotary evaporation to give a mixture of ethyl 2-(4-methyl 2-fluorophenyl)-2,2-difluoroacetate as a yellow liquid of 310 mg. Used directly in the next step of the reaction.

The synthetic route of 452-79-9 has been constantly updated, and we look forward to future research findings.

Related Products of 7681-82-5, 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 7681-82-5 as follows.

General procedure: Nal (2.15 eq.) is added at room temperature to a suspension of PtCI2(1-R-1 ,5-COD)] (1.00 eq.; synthesized as described in Example 1 ) in acetone. The color of the reaction mixture initially turns yellow and the mixture is stirred for three hours. Afterwards the acetone is removed under reduced pressure and the resulting residue is dissolved in a mixture of dichloromethane and water (1 :1 ). The phases are separated and the organic phase is washed twice with water, dried over sodium sulfate and filtered. After removal of the solvent under reduced pressure, the desired Ptl2(1-R-1 ,5-COD) complex can be obtained as a bright yellow to orange solid or wax.50.0 mg (1 .00 eq., 0.128 mmol) [PtCI2(Me-COD)] and 43.2 mg (2.15 eq., 0.258 mmol) Nal in 3 mL acetone were stirred together for three hours. 71.1 mg (0.126 mmol, 97%) of the desired product could be obtained as yellow solid. – Decomposition temperature: >170 C. – 1H-NMR (400 MHz, CDCI3): delta (ppm) = 1.70- 1.90 (m, 1 H, CH2), 1.90-2.20 (m, 3 H, CH2), 2.08 (s d,2JPtH= 20.7 Hz, 3 H, CH3), 2.20- 2.40 (m, 2 H, CH2), 2.50-2.61 (m, 1 H, CH2), 2.61-2.80 (m, 1 H, CH2), 5.56-6.02 (m, 3 H, CH). -13C-NMR (100 MHz, CDCI3): delta (ppm) = 29.8 (-, CH2), 31 .9 (-, CH2), 32.3 (+, CH3), 32.5 (-, CH2), 36.2 (-, CH2), 99.5 (+, CH), 99.7 (+, CH), 101.1 (+, CH), 128.9 (Cquart). – 195Pt-NMR (129 MHz, CDCl3): delta (ppm) = -4240 (s). – IR (ATR) [cm-1]: v-1= 3000 (vw), 2940 (vw), 2874 (vw), 2825 (vw), 2108 (vw), 1718 (vw), 151 1 (vw), 1492 (vw), 1477 (vw), 1423 (w), 1368 (vw), 1347 (vw), 1335 (vw), 1312 (w), 1237 (vw), 1210 (vw), 1 191 (vw), 1 169 (vw), 1 142 (vw), 1095 (w), 1061 (vw), 1036 (vw), 1022 (vw), 1006 (w), 967 (vw), 939 (vw), 895 (vw), 874 (w), 853 (vw). – MS (70 eV, El), m/z (%): 574/572/571/570 (10/45/60/50) [M+], 445/444/443/442/441 (25/30/36/1 1/15) [M+- l], 316/315/314/313/312/31 1/310 (1 1 Pi 8/12/18/12/17/12) (13/23/76/84/86/55/60/36/38/28/13) [M+-2 I], 122 (52) [C9H14+], 107 (39) [CeHu*], 94 (41 ), 68 (100). – HRMS (Ptl2C9H14): calc. 570.8833; found 570.8831. – EA (Ptl2C9H14): calc. C 18.93, H 2.47; found C 19.70, H 2.58.

According to the analysis of related databases, 7681-82-5, the application of this compound in the production field has become more and more popular.

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. 6940-76-7, name is 1-Chloro-3-iodopropane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of 1-Chloro-3-iodopropane

3,4-Dihydroquinolin-2(1 H)-one (2.0 g, 13.6 mmol) dissolved in acetonitrile (10 mL) at 25 C, Cs2C03 (13.0 g, 40.8 mmol) was added and the reaction was stirred at 60C for 1 h then cooled to at 25 C. 1-Chloro-3-iodopropane (3.61 g, 17.7 mmol) was then added and the resulting reaction mixture was stirred at 80C for 48 h. After this time, the reaction mixture was partitioned between cold H20 (150 mL) and EtOAc (100 mL), the aqueous layer was further extracted with EtOAc (2 x 100 mL), the organic layers were combined, dried (Na2S0 ), solvents were removed in vacuo and the residue was purified by column chromatography (Normal silica, mesh size: 60-120, 20.0 % to 25.0 % EtOAc in Hexane) to give 1 -(3-chloropropyl)-3,4- dihydroquinolin-2(1 H)-one (1 .48 g, 48.84 %) as yellow gum. The data for the title compound is in Table 2.

The synthetic route of 6940-76-7 has been constantly updated, and we look forward to future research findings.

Reference of 103962-05-6,Some common heterocyclic compound, 103962-05-6, name is 1-Iodo-4-(trifluoromethoxy)benzene, molecular formula is C7H4F3IO, 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.

Synthesis of 2-oxo- 1 -(4-(trifluoromethoxy)phenyl)- 1 ,2-dihydropyridine-3 – carbaldehyde (2-2) 2-oxo- l,2-dihydropyridine-3-carbaldehyde (200 mg, 1.63 mmdl), 1-iodo- 4-(trifluoromethoxy)benzene 2 (562 mg, 1.95 mmol), 8-hydroxyquinoline (47.2 mg, 0.324 mmol), copper iodide (61.9 mg, 0.324 mmol), and potassium carbonate (303 mg, 2.19 mmol) were combined in a round bottom flask with DMSO (3.5 mL) under a nitrogen atmosphere and heated to 130 °C for 21 h. The reaction was cooled to room temperature and poured into a mixture of 10percent aq. ammonium hydroxide and ethyl acetate. The resultant mixture was filtered through a pad bf Celite and washed with ethyl acetate three times. The layers were separated with the aqueous portion being back extracted with ethyl acetate. The combined organic extracts were washed with brine, dried over Na2S04, and concentrated in vacuo. Purification by flash column chromatography on silica gel (0 – 50percent EtOAc in hexane) gave 92.0 mg (20percent) of 2-2 as an off-white solid: 1H NMR (400 MHz, CDC13) delta 10.34 (1H, d, J= 0.8 Hz), 8.14 (1H, dd, J= 6.9, 2.3 Hz), 7.65 (1H, dd, J= 6.9, 2.3 Hz), 7.45 (2H, m), 7.38 (2H, m), 6.44 (1H, dt, J= 0.8, 6.9 Hz); ESI-MS m/z 284 [C13H8F3NO3 + 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-Iodo-4-(trifluoromethoxy)benzene, its application will become more common.

Adding a certain compound to certain chemical reactions, such as: 886762-71-6, name is 1-Fluoro-3-iodo-2-nitrobenzene, belongs to iodides-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 886762-71-6, Safety of 1-Fluoro-3-iodo-2-nitrobenzene

To a solution of 1-fluoro-3-iodo-2-nitrobenzene (228 mg, 0.854 mmol) in toluene (3 mL) was added potassium carbonate (177 mg, 1.28 mmol) and morpholine (1 mL). The mixture was heated at 85 C for 3 h. The cooled reaction mixture was evaporated and the residue partitioned between EtOAc and water. The aq. phase was extracted with more EtOAc, and the combined organic extracts were washed with water, then brine, dried (Na2SO4) and concentrated in vacuo to leave a residue. FCC (20-50% EtOAc in isohexane) gave the title compound as a light yellow solid (168 mg, 59%). M/z 335 (M+H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Fluoro-3-iodo-2-nitrobenzene, and friends who are interested can also refer to it.

Reference of 10297-05-9,Some common heterocyclic compound, 10297-05-9, name is 1-Chloro-4-iodobutane, molecular formula is C4H8ClI, 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.

4-Chloro-1-(3-pyridyloxy)butane Under a nitrogen atmosphere, a solution of 3-hydroxypyridine (3.50 g, 36.8 mmol) in N, N-dimethylformamide (DMF) (10 mL) was added drop-wise over 5 min to a cold (0-5° C.), stirring slurry of sodium hydride (1.16 g of an 80percent dispersion in mineral oil, 38.6 mmol) in DMF (40 mL). The mixture was allowed to stir and warm to ambient temperature over 1 h. The mixture was then cooled to 0-5° C., and 1-chloro-4-iodobutane (9.67 g, 44.2 mmol) was added drop-wise over 5 min. The resulting dark-brown mixture was stirred at ambient temperature for 2 h. Water (25 mL) was added, followed by saturated NaCl solution (25 mL), and the mixture was extracted with ether (4*50 mL). The combined ether extracts were dried (Na2SO4), filtered, and concentrated by rotary evaporation to a residue that was dried briefly under high vacuum to give 6.89 g (quantitative yield) of an oil.

The synthetic route of 10297-05-9 has been constantly updated, and we look forward to future research findings.

3718-88-5, name is 3-Iodobenzylamine hydrochloride, belongs to iodides-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. Recommanded Product: 3718-88-5

Example 2 Preparation of 2-Chloro-N6 -(3-Iodobenzyl)-9-Methyladenine (6) A solution of 2,6-dichloropurine (4, 2 g, 10.6 mmol), 3-iodobenzylamine hydrochloride (3.14 g, 11.6 mmol), and triethylamine (4.42 mL, 31.7 mmol) in ethanol (20 mL) was stirred for 5 days at room temperature. The resulting solid was filtered, washed with small amount of ethanol, and dried to give compound 5 (2.32 g, 57.0%). 1H NMR (DMSO-d6) delta 4.59 (br d, J=3.5 Hz, 2 H, CH2), 7.13 (pseudo t, J=8.2 and 7.5 Hz, 1 H, H-16), 7.36 (d, J=7.5 Hz, 1 H, H-17), 7.61 (d, J=7.5 Hz, 1 H, H-15), 7.74 (s, 1 H, H-13), 8.14 (s, 1 H, H-8), 8.75 (br s, 1 H, exchangeable with D2O, NH), 13.14 (br s, 1 H, exchangeable with D2O, N9 H). MS (CI NH3) m/z 386 (M+ +1).

The synthetic route of 3718-88-5 has been constantly updated, and we look forward to future research findings.