Iodides-buliding-blocks

Reference of 39959-51-8, 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. 39959-51-8 name is (2-Iodophenyl)methanamine, 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.

General procedure: 2-/3-/4-Iodobenzyl chloride (1a-c) was dissolved in chloroform containing 1.1 equivalents of triethylamine. A solution of substituted benzoyl chloride (2a-g) in chloroform was added dropwise with stirring over 15min. The precipitate that formed was removed by filtration and the resulting filtrate was washed sequentially with water, 1N hydrochloric acid, 5% sodium carbonate and brine. The organic phase was dried over magnesium sulfate (anhyd.), filtered, evaporated to dryness and the resultant 2-/3/-4-substituted-N-(2/3/4-iodo)- benzylbenzamide 3a-i was recrystallized from alcohol. To obtain the corresponding 2-/4-iodo-N-substituted benzyl benzamide derivatives, the same procedure was followed, except that the 2-/4-iodobenzoyl chlorides 2h,2i and isomeric 2-/4-methoxybenzylamines 1d,1e were used. All new compounds 3a-i and 4a-d were characterized by 1H, 13C NMR spectrometry, and elemental analysis or LC-MS.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, (2-Iodophenyl)methanamine, and friends who are interested can also refer to it.

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. 6326-42-7, name is Methyl 2-iodo-4-nitrobenzoate, A new synthetic method of this compound is introduced below., SDS of cas: 6326-42-7

A solution of the compound 8 (10.0 g, 32.57 mmol) and SnCl2. 2 hi) (22.04 g, 97,69 mmol, 3 equiv.) in EtOAc ( 150 mL) was refluxed for 5 hours until TLC (EtOAc/hexane, 1 : 1) indicated that reaction was complete. The reaction mixture was poured in a 500 ml beaker and it was diluted with 100 ml of EtOAc followed by the addition of potassium carbonate and 200 ml of deionized water and the two layer mixture was stirred for 30 minutes. The milky suspension was filtered through a short bed of CELITE and the organic layer was separated. The combined organic layer was sequentially treated with saturated brine and anhydrous Na2S0 . Purification by flash column chromatography using EtOAc: petroleum ether (1 : 1) afforded a pale yellow solid 9 (5.86 g, 65% yield). [0396] FontWeight=”Bold” FontSize=”10″ 1I NMR (400 MHz, CDC13, TMS) delta 3.86 (s, 3H), 4.01 (broad singlet, 2H), 6.58-6.64 (dd, IH, Jj = 2.29 Hz, J2 = 8.70 Hz), 7.30 (d, 1H, J = 2.29 Hz), 7.77 (d, 1H, J – 8.24 Hz). 1 C NMR (100 MHz, CDC13) delta: 51.87, 96.53, 1 13,44, 127,03, 132.95, 150,24, 165,92, MS (ESI): m/z (%) 300. 9 (M Xa }

The synthetic route of 6326-42-7 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. 32024-15-0, name is 3-Iodo-4,5-dimethoxybenzaldehyde, A new synthetic method of this compound is introduced below., COA of Formula: C9H9IO3

(3-Iodo-4,5-dimethoxyphenyl)methanoI (3). A method of Chowdhury and co-workers was modified. A 250 mL, three-necked, round-bottomed flask, equipped with a magnetic stir bar and a condenser was charged with 2 (25 g, 85 mmol) and 100 mL of THF. Sodium borohydride (1.91 g, 50 mmol) was added slowly portion- wise over a period of 5 min and the reaction mixture was stirred at room temperature for 45 min. The reaction mixture was quenched with 100 mL of saturated NH4C1 and extracted with ethyl acetate (3 x 125 mL). The combined organic layers were washed with saturated NaCl (100 mL), dried (MgS04) and concentrated under vacuum to yield 3 (24.8 g, 98.8%) as a thick colorless liquid. IR: 3392, 2824 cm”1; H-NMR(CDC13): delta 7.27 (d, J= 1.6 Hz, 1H), 6.86 (d, J = 1.6 Hz, 1H), 4.53 (s, 2H), 3.83 (s, 3H), 3.79 (s, 3H), 2.83 (br s, 1H); I3C-NMR (CDC13): 5 152.4, 147.7, 139.0, 128.3, 111.2, 92.1, 63.9, 60.3, 55.8.

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.

These common heterocyclic compound, 181765-86-6, name is Methyl 5-bromo-2-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: C8H6BrIO2

Synthesis of Intermediate 1-(6) (0202)3.849 g (11.259 mmol) of methyl 5-bromo-2-iodobenzoate, 3 g (13.510 mmol) of Intermediate 1-(6) (phenanthren-1-ylboronic acid), 30 mL of 2 mol/L potassium carbonate in H2O, and 0.651 g (0.563 mmol) of tetrakis(triphenylphosphine)palladium were added to 100 mL of tetrahydrofuran and 30 mL of methanol under a nitrogen atmosphere and then heat-stirred. After 24 hours, completion of the reaction was confirmed through TLC, and the solvent was removed and filtered using celite. Next, the organic layer was separated using dichloromethane and H2O and washed with a saturated sodium chloride solution. The organic layer was dried with sodium sulfate and filtered. After drying and filtering, the solvent was removed and column chromatography (MC:hexane=1:4) was performed to obtain 3.5 g of Intermediate 1-(6) as a white solid (yield: 79%). (0203) 1H NMR (300 MHz, CDCl3): delta (ppm) 8.80 (d, J=12.6 Hz, 2H), 8.22 (s, 1H), 7.88 (d, J=7.8 Hz, 1H), 7.77 (dd, J=5.1, 1.8 Hz, 1H), 7.737.60 (m, 4H), 7.40 (dd, J=7.8, 1.5 Hz, 2H), 7.32 (d, J=8.1 Hz, 1H), 3.41 (s, 3H) (0204) 13C NMR (75 MHz, CDCl3): delta (ppm) 166.4, 140.7, 139.0, 134.6, 133.5, 133.1, 131.7, 130.3, 130.2, 130.0, 128.5, 127.2, 126.8, 126.7, 125.7, 123.9, 122.9, 122.4, 121.5, 52.1 (0205) A molecular weight for C22H15BrO2: Cal. 390.0255 (0206) LR-Mass (EI+): 392.2, HR-Mass (EI+): 392.0257

The synthetic route of Methyl 5-bromo-2-iodobenzoate has been constantly updated, and we look forward to future research findings.

31599-60-7, name is 1-Iodo-2,3-dimethylbenzene, 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. Formula: C8H9I

General procedure: A suspension of indole-3-carbaldehyde 1 (0.411 g, 2.8 mmol),Cu2O (0.3 equiv), K2CO3 (2.0 equiv) and aryl halide (2.0 equiv) inanhydrous DMF (5.6 mL) was refluxed for 72 h. After cooling to RT,the reaction mixture was filtrated over a celite pad eluting withEtOAc. Solvents were removed and the residue dissolved in EtOAc(20 mL) washed successively by 2.5% aqueous NH4OH, 1 M HCl andsaturated aqueous NaCl. The organic phase was dried over Na2SO4,filtered and concentrated. The residue was purified by flash columnchromatography on silica gel (PE/EtOAc 9:1 to 7:3) to furnish thedesired compound.

The synthetic route of 31599-60-7 has been constantly updated, and we look forward to future research findings.

Application of 452-79-9,Some common heterocyclic compound, 452-79-9, name is 2-Fluoro-1-iodo-4-methylbenzene, molecular formula is C7H6FI, 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 (3S)-piperidin-3-ol hydrochloride (0.50 g, 0.0036 mol), 2-fluoro-l-iodo-4- methylbenzene (1.03 g, 0.00436 mol), copper(I) iodide (140 mg, 0.00073 mol), potassium phosphate (3.08 g, 0.0145 mol), and 1,2-ethanediol (0.810 mL, 0.0145 mol) in 1-butanol (7.28 mL, 0.0796 mol) was heated at 100 0C under nitrogen for 2 nights. The reaction mixture was treated with water, and then extracted with EtOAc. The organic layers were combined, washed with brine, dried and evaporated to dryness. The residue was used directly in next step (519 mg, 69%). LCMS (M+H):210.2.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Fluoro-1-iodo-4-methylbenzene, its application will become more common.

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. 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), A new synthetic method of this compound is introduced below., COA of Formula: C3H6I2

Preparation of 1,3-bis(1-isoquinolyl)-propane 2a; A solution of 2-benzoyl-1-cyano-1,2-dihydroisoquinoline 1a (5.0 g; 19.2 mmol) and of 1,3-diiodopropane (1.1 mL; 9.6 mmol) in DMF (15 mL) was dropwise added to a stirred suspension of sodium hydride (0.46 g; 19.2 mmol) in DMF (30 mL) at -10 C. The content was stirred for 4 h and poured into ice-cold water (200 mL). The creamy solid was filtered off. After drying, the solid was hydrolyzed by treatment with 50% aqueous NaOH in EtOH at reflux. After removal of EtOH, the crude residue was dissolved in ArMe (50 mL) and water (50 mL). The organic layer was collected, washed with water (50 mL) and then extracted with 1N aqueous HCl (2×50 mL). The acidic layers were basified with concentrated NH4OH and finally extracted with CH2Cl2 (3×30 mL). The organic layers were dried over anhydrous MgSO4 and evaporated under reduced pressure to afford a white solid which recrystallized from petroleum ether 100-140 (2.5 g); yield, 40%; mp 96-97 C.1H-NMR (CDCl3) delta 2.49 (pentuplet, 2H, J=7.7 Hz), 3.50 (t, 4H, J=7.7 Hz), 7.51 (d, 2H, J=5.7 Hz), 7.56 (t, 2H, J=7.5 Hz), 7.65 (t, 2H, J=7.5 Hz), 7.80 (d, 2H, J=7.5 Hz), 8.18 (d, 2H, J=7.5 Hz), 8.44 (d, 2H, J=5.7 Hz)Anal. C21H18N2 (298.389) Calc. N, 9.39; C, 84.53; H, 6.08. Found N, 9.56; C, 84.38; H, 6.16.

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 35944-64-0, A common heterocyclic compound, 35944-64-0, name is 3-Iodo-4-methylaniline, molecular formula is C7H8IN, 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 flask containing 1.0 g (2.67 mmol) of 4-[(4-methyl-1 – piperazinyl)methyl]-3-(trifluoromethyl)-benzoic acid (CASNo. 859027-02-4; prepared according to Asaki, T. et a/. Bioorg. Med. Chem. Lett. (2006), 16, 1421-1425), 0.62 g (2.67 mmol) of 3- lodo-4-methylaniline, 0.77 g (4.0 mmol) of N-(3-dimethylaminopropyl)-N’-ethylcarbodiimide hydrochloride (EDAC), and 0.43 g (3.2 mmol) of N-hydroxybenzotriazole monohydrate (HOBt ‘ H2O) was added 5 mL of DCM and 5 mL of triethylamine. The solution was stirred at ambient temperature under an atmosphere of N2 for 3 days, concentrated, and the crude product purified by silica gel chromatography (eluted with 100% EtOAc then 10% MeOH/EtOAc), to provide 0.69 g of product as a white solid.

The synthetic route of 35944-64-0 has been constantly updated, and we look forward to future research findings.

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 54811-38-0 as follows. HPLC of Formula: C8H7IO2

2-methylbenzoic acid as the starting material,Under the action of metal reagent Fe powder and super acid catalyst trifluoromethanesulfonic acid,Adding a liquid bromine having a molar multiple of 1.05,And the solvent solution of bromine absolute molecular sieve without water pretreatment,Synthesis of intermediate 2 5-bromo-2-methyl benzoic acid, the yield of 85% or more

According to the analysis of related databases, 54811-38-0, the application of this compound in the production field has become more and more popular.

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 6940-76-7, name is 1-Chloro-3-iodopropane, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C3H6ClI

A reaction flask was charged with 6,7-difluoro-4H-benzo [1.4]oxazin-3-one (1.5 g, 8.1 mmol), 1-chioro-3-iodopro-pane (1.44 g, 8.1 mmol), and Cs2CO3 (4.0 g, 12.2 mmol) in MeCN (10 mE) and stirred at rt for 40 h. The reactionmixture was concentrated, water added, and the product extracted into EtOAc. The combined organic phases weredried over Na2SO4, filtered, and concentrated. The productwas purified by flash column chromatography (Si02 n-heptane/EtOAc 2:1) to give the title compound (1.88 g, 89%).?H NMR (CDC13) oe 6.99 (dd, J=8.0 Hz, J=5.6 Hz, 1H), 6.79-6.72 (m, 2H), 4.59 (s, 2H), 4.08 (t, J=7.2 Hz, 2H), 3.62(t, J=6.0 Hz, 2H) 2.18-2.10 (m, 2H); ?3C NMR (CDC13) oe163.9, 159.1 (d, J=244.1 Hz), 146.4 (d, J=11.9 Hz), 124.9 (d,J=3.0 Hz), 115.4 (d, J=9.6 Hz), 109.5 (d, J=22.7 Hz), 105.4 (d, J=26.2 Hz), 67.7, 42.4, 39.2, 30.1.

According to the analysis of related databases, 6940-76-7, the application of this compound in the production field has become more and more popular.