Category: iodides-buliding-blocks

Reference of 16355-92-3, The chemical industry reduces the impact on the environment during synthesis 16355-92-3, name is 1,10-Diiododecane, I believe this compound will play a more active role in future production and life.

Example 1 Preparation of 2,2′-(1,12-dodecanediyl)bispyridine LDA (2M) (20 mL, 40.00 mmol) was added dropwise to a solution of 2-picoline (3.73 g, 40.00 mmol) in THF (60 mL) at -78 C. The mixture was stirred for 30 min and then 1,10-diiododecane (6.31 g, 16.00 mmol) in THF (10 mL) was added dropwise. The resulting mixture was warmed to room temperature and stirred for 4 hrs. 50% saturated NH4Cl was added to the reaction mixture. The aqueous phase was extracted with ethylacetate (40 mL*2), and the combined organic liquors were washed with 50% saturated brine (40 mL*3) and saturated brine (40 mL), dried over anhydrous Na2SO4, and concentrated under reduced pressure. The crude product was purified by column chromatography (hexanes:ethylacetate 2:1 to 1:1) to afford 3.75 g of the title compound. Yield: 72%. 1H NMR (300 MHz, CDCl3) delta 1.13-1.42 (m, 16H), 1.60-1.81 (m, 4H), 2.78 (t, J=7.8 Hz, 4H), 7.08 (ddd, J=7.5, 5.1, 0.6 Hz, 2H), 7.13 (d, J=7.5 Hz, 2H), 7.57 (dt, J=7.5, 1.8 Hz, 2H), 8.52 (dd, J=5.1, 0.6 Hz, 2H) ppm; 13C NMR (75 MHz, CDCl3) delta 29.7, 29.75, 29.8, 29.9, 30.2, 38.7, 120.9, 122.8, 136.3, 149.2, 162.5 ppm.

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, 1,10-Diiododecane, other downstream synthetic routes, hurry up and to see.

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 32024-15-0 as follows. Recommanded Product: 3-Iodo-4,5-dimethoxybenzaldehyde

13ax) A mixture of 5.0 g of 3-iodo-4,5-dimethoxy-benzaldehyde, 1.18 g of hydroxylamine hydrochloride, 1.37 g of pyridine and 17 ml of toluene is held at reflux for 2 hrs. (see A. Saednya, Synthesis 1982, 190). The precipitate which separates after cooling is filtered off under suction. Chromatography on silica gel with methylene chloride/methanol 9:1 yields 3.09 g of 3-iodo-4,5-dimethoxy-benzonitrile as a colourless solid. Yield: 63%. Mass spectrum: peaks inter alia at m/e: 289 (100%), 274 (38%), 132 (30%), 119 (43%).

According to the analysis of related databases, 32024-15-0, the application of this compound in the production field has become more and more popular.

Some common heterocyclic compound, 400-97-5, name is 1-Iodo-2-nitro-4-(trifluoromethyl)benzene, molecular formula is C7H3F3INO2, 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. SDS of cas: 400-97-5

To a solution of compound 52 (850 mg, 2.68 mmol) in HOAc- EtOH (10 mL, 1 :5, v/v) was added iron dust (750 mg, 13.43 mmol) at 23 C. The resulting mixture was stirred at 23 C for 3 h before it was quenched with a saturated solution of NaHC03 (20 mL) and diluted with EtOAc (50 mL). The layers were separated, and the organic layer was extracted with H20 (3 x 10 mL). The combined organic layers were dried over Na2SO4 and concentrated in vacuo. The residue was purified by flash column chromatography (silica gel, hexanes: EtOAc 10: 1 ) to give compound 53 (754 mg, 98%) as a yellow solid. (0468) [00359] 1 H NMR (400 MHz, CDCI3) delta = 7.76 (dd, J = 8.2, 0.7 Hz, 1 H), 6.96 (d, J = 1 .7 Hz, 1 H), 6.72 (ddd, J = 8.2, 2.0, 0.6 Hz, 1 H), 4.32 (brs, 2H). m/z (ESI) 288.0 [M+H+].

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 400-97-5, its application will become more common.

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.

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.

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 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.

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. 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.