Category: iodides-buliding-blocks

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.

Related Products of 672-57-1, 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 672-57-1 as follows.

12336] Three point eight (3.8) ml of n-butyllithium (2.6 M hexane solution) was added dropwise to a mixture of 3.00 g of 1 -chloro-2-iodo-4-(trifluoromethyl)benzene and 15 ml oftetrahydrofuran at -70 C., followed by stirring for 30 minutes. Thereafier, a mixture of 1.69 g of N-methoxy-N-methyltrifluoroacetamide and 5 ml of tetrahydrofuran was added drop- wise thereto at -70 C. Subsequently, afier the reaction mixture was stirred for 1 hour at room temperature, water was added thereto, and extraction was performed using ethyl acetate. The organic layer was washed with saturated saline, dried over magnesium sulfate, and then concentrated under reduced pressure. The residues were subjected to silica gel column chromatography, thereby obtaining 1.66 g of 2,2,2- trifluoro-1 -[2-chloro-5-(trifluoromethyl)phenyl]ethanone.

According to the analysis of related databases, 672-57-1, the application of this compound in the production field has become more and more popular.

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.

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. 31928-47-9, name is 4-Bromo-2-chloro-1-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C6H3BrClI

A mixture of Xantphos (1.20 g, 2.05 mmol) and tris(dibenzylideneacetone)dipalladium (0) (1.26 g, 1.37 mmol) in anhydrous anisole (76 mL) was stirred under nitrogen, at 50 0C for 30 minutes to provide a an orange- brown solution of the catalyst.[00326] To a stirred mixture of 6-amino-7-fluoro-3-methyl-3H-benzoimidazole-5- carboxylic acid methyl ester (6) (8.00 g, 34.16 mmol) and cesium carbonate (22.48 g, 68.31 mmol) in anhydrous anisole (76 mL) under nitrogen was added 4-bromo-2- chloroiodobenzene (1.60 g, 1.10 equiv., 4.88 mmol). The preformed catalyst, as prepared above, was then added to the mixture to provide a dark brown suspension, which was heated at 100 +/- 2 0C, with stirring at 350 rpm. The reaction was monitored by HPLC analysis. After 41 hours, no 6-amino-7-fluoro-3-methyl-3//-benzoimidazole-5-carboxylic acid methyl ester (6) remained. The reaction mixture was cooled to about 80 0C and IM sulfuric acid (40.99 mL 40.99 mmol) was added. Gas evolution was observed after 10 minutes and the rate of addition was controlled to moderate the effervescence. At the end of the addition the pH was between 7 and 8. Additional sulfuric acid (IM, 10.25 mL, 10.25 mmol) was then added to give mobile slurry with a pH of 0. The mixture was diluted with anisole (20 mL) and Celatom FW- 14 filter agent was added. It was then filtered at about 80 C through a water-wet pad of Celatom FW- 14 filter agent and the cake was washed with anisole (1 x 40 mL + 3 x 20 mL), then water (10 mL). The lower aqueous layer was separated and discarded and the organic layer was washed with 10 % aqueous NaCl solution (2 x 40 mL). This was added to a sodium hydroxide (5.46 g, 68.3 mmol) in methanol (24 mL) and the mixture was heated at 65 C with stirring. After 17.5 hours HPLC analysis indicated that the hydrolysis of the ester was complete and the slurry was cooled to 15 C, then filtered on a sinter. The solid was washed with water (4 x 24 mL), MTBE (24 mL), and acetonitrile (2 x 25 mL) and then dried at 45 0C in a vacuum oven to provide 11.07 g of 6-(4- EPO bromo-2-chlorophenylamino)-7-fluoro-3-methyl-3H-benzoimidazole-5-carboxylic acid (7) as a fine pale brown solid (assay 93.7% by 1H NMR), actual wt 10.37 g (72.2% yield). 1H NMR (400 MHz, d6 DMSO) delta 3.85 (3H, s, NMe), 6.53 (IH, dd, J 9, 7, Ar-H), 7.27 (IH, dd, J 9S 2.5, Ar-H), 7.56 (IH, d, J 9, Ar-H), 7.97 (IH, s, Ar-H), 8.20 (IH5 s, Ar-H), 11.5 (IH, s, CO2H). 13C NMR (100 MHz, d6 DMSO) delta 31 (CH3), 108 (CH, d, J 2), 109 (CH), 117 (C, d, J6), 122 (C), 124 (C, d, J7), 127 (C)5 130 (C)5 131 (C), 132 (C, d, J9), 133 (C5 d, J l l), 141 (C), 145 (CF, d5 J 252), 146 (CH)5 170 (C=O).

According to the analysis of related databases, 31928-47-9, the application of this compound in the production field has become more and more popular.

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.

These common heterocyclic compound, 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), 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. Recommanded Product: 1,3-Diiodopropane(stabilized with Copper chip)

Examples 13 -22; Synthesis of PBD dimers linked at the C-8 position; n=3, 4,5, 6, 7, 8,9, 10, 11, 12 Example 13 (n=3); (a) 1,1′-[(Propane-1,3-diyl)dioxy]bis[(11S,11aS)-10-(tert- butyloxycarbonyl)-7-methoxy-l1- (tetrahydro-pyran-2-yloxy)- 1,2, 3, 10, 11, IIa-hexahydro-5H-pyrrolo (2, 1-cJ [l, 4] benzodiazepine-5- one] (15a); 1,3-Diiodopropane (66 mg, 0.22 mmol, 0.5 equiv) was added to the mixture of monomer 14 (0.2 g, 0.44 mmol, 1. 0 equiv) and potassium carbonate (0. 98mmol, 2.2 equiv) in dry DMF (30 mL), and the resulting mixture was heated to 90C under a nitrogen atmosphere for 5 h. Removal of excess solvent under reduced pressure afforded a crude solid, which was subjected to flash column chromatography (SiO2, 50% EtOAc-hexane) to afford the dimerized compound 15a (90 mg, 0.09 mmol, 43% yield, mixture of diastereomers from THP protecting group) as a solid: [a] 20D = +57 (c = 0.14, CHCl3); 1H NMR (CDC13, 400 MHz): 5 1. 20-1. 84 (m, 60H, Boc, THP), 1.91-2. 20 (m, 16H, 1-H, 2-H), 2.34-2. 46 (m, 4H, 13-H), 3.40-3. 74 (m, 16H, 3-H, lla-H, THP), 3.79-3. 99 (m, 16H, 7-OMe, THP), 4.12-4. 30 (m, 8H, 12- H), 4.97-5. 15 (m, 4H, THP), 5.66-5. 75 (d, 2H, 11-H), 5. 77-5.89 (d, 2H, 11-H), 6.55 (s, 2H, 9-H), 6.89 (s, 2H, 9-H), 7.16 (s, 2H, 6- H), 7.20 (s, 2H, 6-H) ; 13C NMR (CDCl3, 400 MHz): 6 19.9, 20.5, 23. 1,23. 2,25. 2,25. 3,28. 1,28. 2,28. 9,29. 0, 29. 1,30. 9,31. 3, 46.3, 56.0, 56.1, 60.0, 60.2, 63.4, 64.5, 65.3, 65.7, 81.0, 81.1, 88. 1,91. 2,95. 7,100. 3,110. 1,110. 8, 114.7, 115.2, 127.5, 129.8, 148.5, 148. 8, 150.0, 155.1, 167.4, 167.6 ; IR (neat): 3426, 2943, 1703, 1643,1604, 1513, 1454,1432, 1326,1270, 1201,1163, 1023cm~ r MS (FAB) m/z (relative intensity) 959 ([M + Na]+., 100), 937 (M 62), 835 (67), 735 (60).

The synthetic route of 1,3-Diiodopropane(stabilized with Copper chip) has been constantly updated, and we look forward to future research findings.