Tag: M.W=200-300

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.

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.

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 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.

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.

61272-76-2, name is 4-Fluoro-2-iodoaniline, 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. category: iodides-buliding-blocks

General procedure: A 25mL oven-dried Schlenk tube were added 2-iodoaniline 1a (110mg, 0.5mmol), phenylacetic acid 2a (81.7mg, 0.6mmol) or benzyl chloride 4a (75.9mg, 0.6mmol), selenium powder (118mg, 1.5mmol), CuBr (7.17mg, 10mmolpercent), KOH (56.1mg, 1.0mmol) or Cs2CO3 (326mg, 1.0mmol), DMSO (1.5mL). The tube was purged with nitrogen three times. Then the reaction mixture was stirred in a preheated oil bath at 120°C for 18h. After the reaction was completed, the mixture was diluted with a saturated solution of Na2CO3 (15mL) and extracted with ethyl acetate (3×10mL). The organic layer was dried over anhydrous Na2SO4, then concentrated in vacuo. The residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate, 100/1) to give pure product 3aa.

The synthetic route of 61272-76-2 has been constantly updated, and we look forward to future research findings.

202865-85-8, name is 1-Bromo-4-iodo-2-methylbenzene, 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. Application In Synthesis of 1-Bromo-4-iodo-2-methylbenzene

Step 1 tert-Butyl N-[(3S)-1-(4-bromo-3-methylphenyl)-5-oxopyrrolidin-3-yl]carbamate A suspension of 2-bromo-5-iodotoluene (1.5 g), tert-butyl ((S)-5-oxopyrrolidin-3-yl)carbamate (2.7 g), copper iodide (95 mg), cesium fluoride (1.9 g), and N,N-dimethylethylenediamine (0.11 ml) in acetonitrile (20 ml) was stirred at 100 C. for 3 hours under a nitrogen atmosphere. After cooling, a saturated aqueous solution of ammonium chloride was added to the reaction solution, followed by extraction with ethyl acetate. The extract was washed with a 10% aqueous sodium thiosulfate solution and saturated saline in this order and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel column chromatography (chloroform-methanol) to obtain the title compound (1.8 g). 1H-NMR (CDCl3) delta: 1.45 (9H, s), 2.40 (3H, s), 2.47 (1H, dd, J=17.2, 4.5 Hz), 2.96 (1H, dd, J=17.2, 8.2 Hz), 3.69 (1H, d, J=9.7 Hz), 4.13 (1H, dd, J=9.7, 6.7 Hz), 4.41 (1H, br s), 4.83 (1H, br s), 7.29 (1H, d, J=8.5 Hz), 7.47-7.52 (2H, m).

The synthetic route of 202865-85-8 has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 204257-72-7, name is Methyl 2-fluoro-4-iodobenzoate, 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. Formula: C8H6FIO2

4-[(8-Cyclopropyl-3,4-dihydro-4,4-dimethylspiro[2H-1-benzopyran-2.1′-cyclopropane]-6-yl)ethynyl]-2-fluoro-benzoic acid methyl ester (Compound 53, General Formula 1) Following general procedure F and using 8-cyclopropyl-6-ethynyl-3,4-dihydro-4,4-dimethylspiro[2H-1-benzopyran-2,1′-cyclopropane] (Intermediate 44, 0.03 g, 0.11 mmol), methyl-2-fluoro-4-iodo-benzoate (Reagent G, 0.025 g, 0.09 mmol), triethyl amine (3 mL), tetrahydrofuran (3 mL), copper(I)iodide (0.020 g, 0.1 mmol) and dichlorobis(triphenylphosphine)palladium(II) (0.06 g, 0.085 mmol) followed by preparative normal phase HPLC using 10% ethyl acetate in hexane as the mobile phase, the title compound was obtained as a white solid (0.019 g, 40%). 1H NMR (300 MHz, CDCl3): delta 7.97 (t, 1H, J=7.8 Hz), 7.34 (d, 1H, J=1.9 Hz), 7.32-7.25 (m, 2H), 6.83 (d, 1H, J=1.9 Hz), 3.95 (s, 3H), 2.06-1.96 (m, 1H), 1.93 (s, 2H), 1.42 (s, 6H), 1.06-1.02 (m, 2H), 0.91-0.86 (m, 2H), 0.71-0.61 (m, 4H).

The synthetic route of Methyl 2-fluoro-4-iodobenzoate has been constantly updated, and we look forward to future research findings.

Reference of 10297-05-9, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 10297-05-9 name is 1-Chloro-4-iodobutane, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

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-chloro4-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.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Chloro-4-iodobutane, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 58313-23-8, name is Ethyl-3-iodobenzoate, 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 58313-23-8, COA of Formula: C9H9IO2

General procedure: A dry and argon-flushed Schlenk tube, equipped with a magnetic stirring bar and a rubber septum was charged with Ni(acac)2 (12.8 mg, 0.05 mmol, 0.05 equiv) as catalyst, 4-fluorostyrene (24.4 mg, 0.20 mmol, 0.20 equiv), the aryl iodide or heteroaryl chloride 3 as electrophile (1.00 mmol, 1.00 equiv), and freshly distilled THF (1 mL). The resulting suspension was cooled to 0 C and the prior prepared benzylic manganese chloride solution (1.20 mmol, 1.20 equiv) was added dropwise at the prior adjusted temperature. The reaction conversion was monitored by GC analysis of hydrolyzed aliquots. After full conversion of the selected electrophile, the reaction mixture was quenched with a sat. aq NH4Cl and extracted with EtOAc (3 × 75 mL). The combined organic layers were dried (MgSO4), filtered, and concentrated under reduced pressure. Purification of the crude product by flash column chromatography afforded the desired products.

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