Iodides-buliding-blocks

Electric Literature of 628-77-3,Some common heterocyclic compound, 628-77-3, name is 1,5-Diiodopentane, molecular formula is C5H10I2, 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.

Sodium hydride (9.73 mg, 0.243 mmol, 60%> suspension in mineral oil) was added to a solution of l ,3-difluoro-2-(((l ,l ,l ,3,3,3-hexafluoro-2-(4-(((4- fluorophenyl)sulfonyl)methyl)phenyl)propan-2-yl)oxy)methyl)benzene (13.2 mg, 0.024 mmol) and 1 ,5-diiodopentane (31.5 mg, 0.097 mmol) in Nu,Nu-dimethylformamide (1 mL). After 1 h at room temperature, LCMS analysis showed that the reaction was complete. The mixture was quenched with water (1 mL), diluted with ether (10 mL), washed with water (2×10 mL), brine (5 mL), dried (magnesium sulfate), filtered and concentrated under reduced pressure. The crude material was purified via preparative LC/MS with the following conditions: Column: Waters XBridge C18, 19 x 150 mm, 5-muiotaeta particles; Guard Column: Waters XBridge C I 8, 19 x 10 mm, 5-muiotaeta particles; Mobile Phase A: 5 :95 acetonitrile: water with 10-mM ammonium acetate; Mobile Phase B: 95 :5 acetonitrile: water with 10-mM ammonium acetate; Gradient: 60-100% B over 15 minutes, then a 5-minute hold at 100% B; Flow: 20 mL/min. Fractions containing the desired product were combined and dried via centrifugal evaporation to give Example 1 (9.0 mg, 57% yield). LC/MS (M+18): 628.1 ; LC retention time: 3.130 min (analytical HPLC Method C); 1H NMR (500 MHz, 1 : 1 mixture of CDC13-CD30D) delta ppm 7.66 – 7.58 (m, 2H), 7.49 – 7.38 (m, 3H), 7.30 – 7.21 (m, 2H), 7.08 – 6.95 (m, 4H), 4.73 (s, 2H), 2.66 (d, J=12.9 Hz, 2H), 2.26 (td, J=13.3, 3.2 Hz, 2H), 1.83 (d, J=13.4 Hz, 2H), 1.67 (d, J=12.4 Hz, 1H), 1.47 – 1.34 (m, 1H), 1.28 (q, J=13.0 Hz, 2H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,5-Diiodopentane, 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. 4387-36-4, name is 2-Iodobenzonitrile, A new synthetic method of this compound is introduced below., Formula: C7H4IN

Example 19 3-[2-({4-[(2,4-difluorophenoxy)methyl]phenyl}sulfonyl)plienyl]-4/r-l,2,4-triazole Step 1: 2-JOdO-JV -4H- l,2,4-triazol-4-ylbenzenecarboximidamide; 4H-l,2,4-Triazol-4-amine (5.0 g, 0.06 mol) and 2-iodobenzonitrile (13.6 g, 0.06 mol) were added to sodium ethoxide (21percent in ethanol, 0.06 mol) and heated to 78 0C for 5 h. The cooled reaction mixture was poured into water and the resulting precipitate filtered off and azeotroped with toluene to give the title compound as a solid (15.6 g, 81percent). 1H NMR (400 MHz, DMSO): delta 8.40 (2 H, s), 7.92 (1 H, d, J 7.6 Hz), 7.51-7.43 (3 H, m), 7.37 (1 H, d, J 4.3 Hz), 7.25-7.19 (1 H, m).

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.

Electric Literature of 7425-53-8, The chemical industry reduces the impact on the environment during synthesis 7425-53-8, name is Ethyl 4-iodobutanoate, I believe this compound will play a more active role in future production and life.

Add K2S2O5(3.0 equiv), Na2HPO4(2.0 equiv) and p-phenylstyrene (0.2 mmol) to thereaction tube in sequence, replace the air in the test tube with high-purity nitrogen and add 2 mL of DMF Solvent.Then, ethyl 4-iodobutyrate (4.0 equiv), triisopropylsilane (2.0 equiv) were added sequentially with a micro sampler, and stirred at 50 C for 24 hours.After the reaction was completed, the reaction solution was diluted with EA, extracted with water and saturated brine, respectively, and then the organic layer was dried, concentrated and separated by column chromatography to obtain the corresponding 1,2-bissulfone group-substituted compound 3c in 58% yield.

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, Ethyl 4-iodobutanoate, other downstream synthetic routes, hurry up and to see.

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. 620-05-3, name is (Iodomethyl)benzene, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 620-05-3

General procedure: A mixture of benzyl bromide (171 mg, 1 mmol), diphenyl disulfide (131 mg, 0.6 mmol), PPh3 (184 mg, 0.7 mmol), and [pmIm]Br21 (94 mg, 0.4 mmol) was stirred at 75 C for 1.5 h (TLC). The reaction mixture was extracted with Et2O, and the organic layer was washed with brine (2 × 5 mL) and dried (Na2SO4). Evaporation of solvent left the crude product which was purified by column chromatography over silica gel (hexane) to afford the pure product, benzyl phenyl sulfide (168 mg, 84%) as a colorless liquid; IR (neat) 3058, 3028, 2923, 1581, 1495, 1479, 1452, 1438, 1238, 1090, 1068, 1024 cm-1; 1H NMR (300 MHz, CDCl3) delta 4.21 (s, 2H), 7.32-7.41 (m, 10H); 13C NMR (75 MHz, CDCl3) delta 39.5, 127.6, 128.0, 129.0 (2C), 129.3 (2C), 129.5 (2C), 130.3 (2C), 136.9, 137.9. The spectroscopic (FT-IR, 1H NMR and 13C NMR) data are in good agreement with the reported values.9b The remaining ionic liquid was washed with ether, dried under vacuum, and reused five times without appreciable loss of catalytic activity.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 620-05-3.

Electric Literature of 5876-51-7,Some common heterocyclic compound, 5876-51-7, name is 5-Iodobenzo[d][1,3]dioxole, molecular formula is C7H5IO2, 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.

[00200] To 21.9 mg NiCl2(dppf) in a reaction tube under nitrogen were added 4 ml dioxane, 0.42 ml (3 mmol) triethylamine, 0.22 ml (1.5 mmol) pinacolborane and 238 mg (0.96 mmol) 1-iodo-3,4-methylenedioxybenzene. The green coloured reaction solution was warmed to 80 C. with stirring for 6 h in an oil bath. An aliquot (ca. 0.3 ml) of the reaction solution was removed, extracted into diethyl ether and washed several times with water and analysed by gc (fid detector, SGE HTS capillary column). Besides a little 1,3-benzodioxole, the only other product peak in the gc was that due to the desired arylboronic acid pinacol ester. NiCl2 (dppf) was also shown to catalyse the formation of the desired product in acetonitrile.

The synthetic route of 5876-51-7 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 766-99-4 as follows. HPLC of Formula: C8H5I

To a solution of l-ethynyl-4-iodobenzene 6 (0.908 g, 3.98 mmol) in THF (20 mL) at -78 0C was added ethylmagnesium bromide (3M in ether, 1.39 mL, 4.18 mmol). After 10 minutes the cooling bath was removed and the solution was allowed to stir at room temperature for 1 hour. The reaction mixture was then re- cooled to 0 0C and added to a solution of N-(tert-butoxycarbonyl)-L-proline N’- methoxy-N’-methylamide 2 (0.970 g, 3.76 mmol) in THF (10 mL). The reaction mixture was warmed to room temperature and stirring was continued for 12 hours before the mixture was quenched with saturated NH4Cl. The mixture was diluted with ethyl acetate/H2O, the layers separated and the aqueous phase was re-extracted with ethyl acetate (2x). The combined organic layers were washed (H2O, brine), dried (Na2SO4), and filtered, and the solvent was removed in vacuo. The resulting residue was purified by flash chromatography (hexane: ethyl acetate, 4: 1) to give (S)- tert-butyl 2-(3-(4-iodophenyl)propioloyl)pyrrolidine-l-carboxylate 7 (0.908 g, 71%) as a yellow oil which solidified on standing. 1H NMR (400 MHz, CDCl3) delta 7.72 – 7.76 (m, 2H), 7.26 -7.30 (m, 2H), 4.49 (dd, J=S. S, 4.3 Hz, 0.3H), 4.29 (dd, J=8.5, 5.5 Hz, 0.7 H), 3.59 (app t, J=6.7 Hz, 2H), 2.20 – 2.33 (m, IH), 1.85 – 2.10 (m, 3H), 1.45, 1.40 (s, 9H, rotamers in 2:3 ratio). LCMS: Anal. Calcd. for Ci8H20INO3: 425; found: 326 (M+H-Boc)+.

According to the analysis of related databases, 766-99-4, 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. 146137-72-6, name is 2-Fluoro-6-iodobenzaldehyde, This compound has unique chemical properties. The synthetic route is as follows., Formula: C7H4FIO

Step 2: To a solution of 2-fluoro-6-iodobenzaldehyde (1.5 g, 6.0 mmol) and 2-bromopyridine-3, 4- diamine (1.1 g, 6.0 mmol) in ethanol (20 mL), was added ferric chloride (778 mg, 4.80 mmol). The reaction mixture was stirred at 60 C under oxygen atmosphere overnight. The next day, solvent was evaporated via rotavap and theresulting residue was purified by column chromatography on silica gel eluting with petroleum/ethyl acetate (3 :1) to give the desired product (1.6 g, 64% yield) as a yellow solid. LCMS (ESI) m/z: 418 [M+H+].

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 146137-72-6.

Electric Literature of 620621-48-9, A common heterocyclic compound, 620621-48-9, name is Methyl 2-chloro-5-iodobenzoate, molecular formula is C8H6ClIO2, 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.

8.1 2-Chloro-5-(pyrimidin-4-ylamino)-benzoic acid methyl ester Sodium phenoxide (810 mg), tris(dibenzylideneacetone)dipalladium (0) (102 mg), Xantphos (161 mg) and methyl-2-chloro-5-iodobenzoate (1379 mg) were placed in a flask and flushed with argon. 4-aminopyrimidine (486 mg) and dioxane (27.5 mL) were added and the reaction mixture was heated to 120 C. for 18 h. After cooling to RT, it was diluted with EtOAc and washed with a 1M solution of NaOH. The organic phase was dried over MgSO4 and concentrated in vacuo. The crude material was purified by CC (Hept/EtOAc 1/1 to 0/1) to give 718 mg of the titled compound as a yellowish powder. LC-MS (B): tR=0.48 min; [M+H]+: 264.21.

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.

Electric Literature of 689260-53-5, A common heterocyclic compound, 689260-53-5, name is 2-Bromo-5-iodo-1,3-dimethylbenzene, molecular formula is C8H8BrI, 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.

A mixture of 2-bromo-5-iodo-1,3-dimethylbenzene (300 mg, 0.965 mmol), 1-aminocyclopropane carboxylic acid (195 mg, 1.93 mmol), copper iodide (I) (37 mg, 0.194 mmol), and diazabicycloundecene (0.50 mL, 3.35 mmol) in dimethylacetamide (2.6 mL) was stirred at 120C for three hours under nitrogen atmosphere. The reaction mixture was purified by silica gel column chromatography (Wakosil C18, acetonitrile – water (0.1% formic acid)) to afford 1-((4-bromo-3,5-dimethylphenyl)amino)cyclopropane carboxylic acid (219 mg, 80%). MS(ESI) m/z = 284, 286 (M+H)+.

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.

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 916792-62-6 as follows. Formula: C7H3FIN

Intermediate 50: 3-Fluoro-2-(pyrimidin-2-yl)benzoic acid.Step A: 3-Fluoro-2-(pyrimidin-2-yl)benzonitrile. 2-lodo-3- fluorobenzonitrile (2.5 g, 10.3 mmol) and 2-tributylstannane pyrimidine (3.7g, 10.0 mmol) were combined and dissolved in degassed DME (18 ml) then purged with bubbling N2 for 5 minutes. The reaction was treated withPd(PPh3)4 (577 mg, 0.5 mmol) and then purged with bubbling for 5 minutes in a sealed vessel and then heated in microwave at 160 C for 90 min. The reaction was cooled and filtered through celite and concentrated to minimum volume and the ppt the formed was diluted with hexanes (40 ml) and cooled to 0 C then filtered. The solid purified (FCC) (20-100% EA / hex) to give 3-fluoro- 2-(pyrimidin-2-yl)benzonitrile. 1 H NMR (400 MHz, CDCI3): 8.93 (d, J = 4.9 Hz, 2H), 8.14 (dd, J = 9.6, 2.7 Hz, 1 H), 7.86 (dd, J = 8.6, 5.3 Hz, 1 H), 7.36 (t, J = 4.9 Hz, 1 H), 7.32 – 7.24 (m, 1 H).

According to the analysis of related databases, 916792-62-6, the application of this compound in the production field has become more and more popular.