Category: iodides-buliding-blocks

Adding a certain compound to certain chemical reactions, such as: 16355-92-3, name is 1,10-Diiododecane, 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 16355-92-3, Formula: C10H20I2

2,15-hexadecanedione as an aliphatic diketone was synthesized. In a 2 L four-necked flask equipped with a thermometer, mixer and a reflux condenser, 260.3 g (2.0 mol) of ethyl acetoacetate and 500 ml of acetone were fed, stirred and mixed, 61.9 g (1.5 mol) of 97% sodium hydroxide was added and reacted for 15 minutes. Then 197.0 g (0.5 mol) of 1,10-diiododecane was added and the reaction was carried out under reflux for 6 hours. After completion of the reaction, acetone was distilled off by distillation under reduced pressure, neutralized by adding 2N hydrochloric acid, and separation was carried out. The upper layer organic layer was separated and 800 g (2.0 mol) of 10% sodium hydroxide aqueous solution was added and stirred at room temperature for 8 hours to carry out a saponification reaction, 205.8 g (1.1 mol) of 50% sulfuric acid was added, and the mixture was fully refluxed for 3 hours for decarboxylation reaction. After the decarboxylation reaction was completed, the upper organic layer was separated by phase separation and cooled to room temperature to obtain 130.8 g of a pale yellow crystal. A small amount of a part of the obtained crystal product was taken for gas chromatograph measurement. As a result of analyzing the composition of the separated crystals by gas chromatography, the conversion of 1,10-diiododecane was 100%, the purity of 2,15-hexadecanedione was 92%.The yield of 2,15-hexadecanedione based on 1,10-diiododecane was 95%

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,10-Diiododecane, and friends who are interested can also refer to it.

Synthetic Route of 1271523-34-2, A common heterocyclic compound, 1271523-34-2, name is 1,5-Dichloro-2-iodo-3-methoxybenzene, molecular formula is C7H5Cl2IO, 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 solution of 11a (21.0g, 69.3mmol) in THF (250ml) was sequentially added Cul (1.32g, 6.9mmol) and NaH (60% dispersion in mineral oil, 4.2g, 104mmol), followed by a slow addition of pinacolborane (15.1ml, 104mmol). The resulting suspension was stirred at room temperature for 16 h under a N2 atmosphere, and then quenched with saturated NH4CI (250 ml). After 20 min, the mixture was extracted with EtOAc (x3), dried and then filtered over Celite. Concentrated and purification by column chromatography (Si02; EtOAc:PE 0: 1?3:7) to afford the title boronate as a white solid; (15. lg, 72%)NMR (CDC13) 6.87 (IH, d, J 1.6), 6.63 (IH, d, J 1.6), 3.37 (3H, s), 1.32 (12H, s);MS (m/e) No MI observed, Rt 1.17min (QC Method 2)

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.

Application of 2974-94-9, These common heterocyclic compound, 2974-94-9, name is 1-Iodo-4-phenoxybenzene, 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.

Example 2A 3-(4-phenoxyphenoxy)quinuclidine 3-Hydroxy quinuclidine (Aldrich, 254 mg, 2 mmol) was treated with 1-iodo-4-phenoxy-benzene (Aldrich, 296 mg, 1 mmol), Cul (Strem Chemicals, 19 mg, 0.1 mmol), 1,10-phenanthroline (Aldrich, 36 mg, 0.2 mmol), and Cs2CO3 (660 mg, 2.0 mmol) in toluene (anhydrous, Aldrich, 10 mL) and heated at 110 C. for two days. After cooling to room temperature, the reaction mixture was diluted with ethyl acetate (50 mL) and washed with water (2*10 mL). The organic phase was concentrated and the title compound was purified by chromatography (SiO2, CH2Cl2:MeOH:NH3H2O, 90:10:1, Rf. 0.20) as oil (220 mg, yield, 75%). 1H NMR (MeOH-d4, 300 MHz) delta 1.45-1.58 (m, 1H), 1.64-1.85 (m, 2H), 2.00-2.15 (m, 1H), 2.20-2.30 (m, 1H), 2.70-3.10 (m, 5H), 3.34-3.40 (m, 1H), 4.52 (m, 1H), 6.83-6.98 (m, 6H), 7.03 (tt, J=7.5, 1.0 Hz, 1H), 7.20-7.41 (m, 2H) ppm. MS (DCl/NH3) m/z 296 (M+H)+.

Statistics shows that 1-Iodo-4-phenoxybenzene is playing an increasingly important role. we look forward to future research findings about 2974-94-9.

Adding a certain compound to certain chemical reactions, such as: 7425-53-8, name is Ethyl 4-iodobutanoate, 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 7425-53-8, SDS of cas: 7425-53-8

Ethyl ester 4-Et. DIEA (11.8 g, 91.7 rnmol) was added to a mixture of compound 3 (13.9 g, 45.87 mmol) and ethyl 3- iodobutyrate (13.3 g, 55.05 minol) in a screw-cup bottle, and the reaction mixture was stirred with heating (110 C) for 2 days. After cooling, the reaction mixture was diluted with diethyl ether, passed through a plug of silica gel (eluting with ether), and the filtrate evaporated in vacuo. The residue was dissolved in hexane/ether (3/1) mixture, washed with water, brine and dried over MgSO4. The product 4-Et was isolated by a short path column chromatography (hexane-hexane/ether 10/1; Rf = 0.59 in hexane/ether = 10/1); yield 18.75 g (98.5%) of a clear oil. ?H NMR (300 MHz, CDC13): delta = 0.21 (s, 6 H, SiMe2But), 0.98 (5, 9 H, SiMe2But), 1.26 Ct, J = 7.2 Hz, 3 H, CO2CH2CH3), 1.28 Cs, 6 H, 2xMe), 1.90 Cm, 2 H, NCH2CH2CH2CO2Et), 1.93 (d, J = 0.5 Hz, 3 H, Me), 2.38 Cm, 2 H, NCH2CH2CH2CO2Et), 3.20 (m, 2 H, NCF{2CH2CH2CO2Et), 4.16 (q, J = 7.2 Hz, 2 H, CO2CH2CH3), 5.10 (d, J = 0.5 Hz, 1 H, HC=), 6.02 Cm, 1 H), 6.10 Cm, 1 H), 6.90 Cm, 1 H) ppm.

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

Electric Literature of 610-97-9, A common heterocyclic compound, 610-97-9, name is Methyl 2-iodobenzoate, molecular formula is C8H7IO2, 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.

General procedure: A 50mL round-bottomed flask equipped with a gas inlet tube, a reflux condenser, and a magnetic stirring bar was charged with MCM-41-S-PdCl2 (173mg, 0.05 mmol Pd), aryl halide (5.0 mmol) and HCOONa (7.5 mmol). The flask was flushed with carbon monoxide. DMF (5 mL) was added by syringe and a slow stream of CO was passed into the suspension. The mixture was vigorously stirred at 100-110C for 4-24h, cooled to room temperature, and diluted with diethyl ether (50 mL). The palladium catalyst was separated from the mixture by filtration, washed with distilled water (2×10 mL), ethanol (2×10 mL) and ether (2×10 mL) and reused in the next run. The ethereal solution was washed with water (3×20mL) and dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by flash column chromatography on silica gel (hexane-ethyl acetate=10:1). (0008) All formylation products were characterized by comparison of their spectra and physical data with authentic samples. IR spectra were determined on a Perkin-Elmer 683 instrument. 1H NMR (400MHz) and 13C NMR (100MHz) spectra were recorded on a Bruker Avance 400MHz spectrometer with TMS as an internal standard and CDCl3 as solvent.

The synthetic route of 610-97-9 has been constantly updated, and we look forward to future research findings.

Reference of 181765-86-6, A common heterocyclic compound, 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, molecular formula is C8H6BrIO2, 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.

Example 5 [00619] Preparation of Cpd 30 [00620] Step A: A mixture of methyl 5-bromo-2-iodobenzoate (18.4 g, 54.0 mmol), TMS acetylene (8.5 mL, 5.88 g, 60.0 mmol), Cul (0.51 g, 2.7 mmol), PdCl2(Ph3P)2 (1.9 g, 2.7 mmol), Et3N (15.0 mL, 10.9 g, 108.0 mmol) and acetonitrile (100 mL) was stirred under argon at room temperature for 4 hours. After the removal of the volatiles in vacuo, the residue was chromatographed (silica gel, ethyl acetate in hexanes, 0-20%) to provide the TMS alkyne intermediate as colorless oil (15.7 g, 94%).

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.

Adding a certain compound to certain chemical reactions, such as: 199786-58-8, name is (5-Bromo-2-iodophenyl)methanol, 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 199786-58-8, Computed Properties of C7H6BrIO

To a stirred solution of PDC (11.0 g, 0.0288 mol) in CH2Cl2 (60 mL) was added a solution of 11 (4.50 g, 0.0144 mol) in CH2Cl2 (20 mL). The mixed content was stirred for 4 h at rt. The solvent was then removed under vacuum to give the crude product of 12, which was purified by silica flash column chromatography (hexanes/CH2Cl2, 7:3) to give compound 12 (4.40 g, 0.0142 mol, 98%) as a white solid.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Application of 52570-33-9, 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. 52570-33-9 name is Methyl 3-iodo-2-methylbenzoate, 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.

Process using Pd Catalyst Under a nitrogen atmosphere, palladium acetate (223 mg, 0.99 mmol) , 4, 5-bis (diphenylphosphino) -9, 9-dimethylxanthene (Xantphos) (575 mg, 0.99 mmol) and toluene (62 ml) were mixed, and the mixture was stirred at room temperature for 15 minutes. To this solution, 2-amino-3-bromo-5-methylpyridine (6.20 g, 33.15 mmol), methyl 3-iodo-2-methylbenzoate (9.15 g, 33.15 mmol) and cesium carbonate (15.12 g, 46.41 mmol) were added. The mixture was stirred at an internal temperature of 100 to 105C for 7 hours. The reaction solution was cooled to room temperature, and water (50 ml) and toluene (50 ml) were added thereto. The organic layer was separated and washed sequentially with water (40 ml) and 10% brine (40 ml) . Silica gel (6 g) was added to the organic layer, the mixture was filtered, and the filtrate was concentrated under reduced pressure. Ethyl acetate (0.5 ml) and n-hexane (6 ml) were added to the concentrate, and the mixture was stirred at room temperature for 30 minutes. The crystals were collected by filtration, washed with ethyl acetate/n-hexane (1/12, 5 ml), and dried under reduced pressure at 40C, to yield the title compound (4.81 g) (yield 43.3%). 1H-NMR (CDCl3, TMS, 300 MHz) delta (ppm) : 2.23 (3H, s) , 2.52 (3H, s), 3.91 (3H, s), 6.78 (IH, brs) , 7.27 (IH, t, J = 8.0 Hz), 7.57-7.62 (2H, m) , 7.95 (IH, d, J = 1.1 Hz), 8.10 (IH, dd, J = 1.0 Hz, 8.1 Hz) .High resolution mass spectrometry Theoretical value: 334.0317 [M+] Measured value: 334.0313 [M+]Melting point: 63.9 to 64.7C

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

Reference of 3930-83-4, These common heterocyclic compound, 3930-83-4, name is 2-Iodobenzamide, 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.

General procedure: To a 25ml Schlenk tube containing a solution of 1 in 2ml of THF was added amide (1.0 mmol) and (EtO)3SiH (0.50 g, 3.0 mmol). The reaction mixture was stirred at 60 C until there was no amide left (monitored by TLC and GC-MS). The product was purified according to literature procedures by Beller [27].

The synthetic route of 3930-83-4 has been constantly updated, and we look forward to future research findings.

Related Products of 21740-00-1,Some common heterocyclic compound, 21740-00-1, name is 5-Bromo-2-iodobenzoic acid, molecular formula is C7H4BrIO2, 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.

A mixture of 5-bromo-2-iodobenzoic acid (2) (800 mg, 2.447 mmol) and 3.5 mL of thionyl chloride was refluxed with stirring for 1 h under a N2 atmosphere, then excess of thionyl chloride was removed in vacuo. Under N2 atmosphere, sodium azide (191 mg, 2.9 mmol) and dry acetone (7 mL) were poured into the flask containing the crude acyl chloride and the mixture was stirred at room temperature for 10 min, after that, acetone was removed in vacuo. CAUTION, the acyl azide is potentially explosive, the solution should not be evaporated to complete dryness. The residue was dissolved in dry toluene (7 mL) and the mixture was stirred at 80-85 C for 3.5 h under a N2 atmosphere. To the reaction flask was added benzyl alcohol (258.0 muL, 2.5 mmol) and 4-dimethylaminopyridine (DMAP, 7.5 mg, 0.06 mmol), the resulting mixture was again stirred at 80-85 C for 1 h under N2 atmosphere. The reaction mixture was diluted with ethyl acetate and after the usual aqueous work up, the organic layer was concentrated to yield a solid residue. This solid was dissolved in dichloromethane and then petroleum ether was added to precipitate the product which was triturated and washed with dichloromethane/petroleum ether mixture to afford (3) 861 mg, 81% yield.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-Bromo-2-iodobenzoic acid, its application will become more common.