Category: iodides-buliding-blocks

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.

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.

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.

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. 41252-95-3, name is 1-Chloro-4-iodo-2-nitrobenzene, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 41252-95-3

A solution of 1-chloro-4-iodo-2-nitrobenzene 4(1) (5.64 g, 0.02 mol) and Na phenylsulfinate 4(2) (3.28 g, 0.02 mol) in DMF (80 ml) was stirred for 12 h at 120 C. Then, the reaction mixture was cooled, poured into water and extracted with ethyl acetate. Organic layer was dried over Na2SO4, filtered and evaporated to dryness. The mixture was separated by means of column chromatography, eluent-ethyl acetate:hexane 1:4. It gave 2.4 g (30.6%) 4-iodo-2-nitro-1-(phenylsulfonyl)benzene 4(3).

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 41252-95-3.

Electric Literature of 58313-23-8, 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. 58313-23-8 name is Ethyl-3-iodobenzoate, 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.

A dry and argon-flushed round-bottomed flask equipped with a magnetic stirring bar was charged with ethyl 3-iodobenzoate (178 mg, 0.64 mmol, 3.75 eq.) in dry THF (1.0 mL) and cooled to -20 C. A solution of isopropylmagnesium chloride-lithium chloride complex (1.3M in THF, 0.33 mL, 0.43 mmol, 2.5 eq.) was added dropwise and the resulting mixture was stirred at – 20 C for 1 h. To the reaction mixture, was then added aldehyde 5 [13] (56 mg, 0.17 mmol) as a solution in THF (0.5 mL, rinsed with an additional 0.5 mL), and the mixture was stirred at – 20 C for 25 min. The reaction was quenched by adding methanol (0.5 mL) and diluting with water (5 mL). The whole mixture was extracted with ethylacetate (20 mL x 3). The combined organic layers were washed with brine (5 mL), dried over sodium sulfate and filtered. Evaporation of the filtrate afforded a residue, from which 6a (68 mg, colorless solid, 86%) was separated by silica gel column chromatography (ethyl acetate: n-hexane 1: 15) as a C22-epimeric mixture (77:23). 6a: 1H NMR (400 MHz, TMS, CDCl3) d – 0.01 (6H x 0.23, s), 0.01 (6H x 0.77, s), 0.70 (3H, d, J 6.8 Hz), 0.88 (9H x 0.23, s), 0.90 (9H x 0.77, s), 0.95 (3H x 0.77, s), 0.96 (3H x 0.23, s), 1.40 (3H, t, J 7.1 Hz), 3.97 (1H x 0.23, s), 4.03 (1H x 0.77, m), 4.38 (2H, q, J 7.2 Hz), 4.89 (1H x 0.23, d, J 3.2 Hz), 4.98 (1H x 0.77, s), 7.41 (1H, t, J 7.7 Hz), 7.51 (1H, d, J 7.7 Hz), 7.92 (1H, d, J 7.7 Hz), 7.95 (1H x 0.77, s), 8.00 (1H x 0.23, s); HRMS (ESI) m/z calcd. for C28H46O4SiNa [MNa] 497.3058, found 497.3060.

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.

Related Products of 13194-68-8, A common heterocyclic compound, 13194-68-8, name is 4-Iodo-2-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.

4-iodo-2-methylbenzenamine 24 (233 mg, 1 mmol) on reaction with 1-tert-butyl-4-ethynylbenzene (25b, 158 mg, 1 mmol) by employing Sonagashira coupling conditions using Pd(PPh3)4 (69.3 mg, 0.06 equiv) as catalyst, Cul (22.8 mg, 0.12 equiv) as cocatalyst, butyl amine (261 mg, 3 equiv) as base and ether as solvent and kept the reaction for 6 h. After completion of the reaction as indicated by TLC and the reaction mixture is extracted into ether (4×25 mL) from the aqueous layer and concentrated in vacuo. The compound was further purified by column chromatography using 60-120 silica gel (ethyl acetate/hexane,1:9) to obtain 4-((4-tert-butylphenyl) ethynyl)-2-methyl benzene amine (26b) as pure product. Anthranilic acid (27, 137 mg, lmmol) on reaction with acetic anhydride at 150 C. and reflux for 30 min, after completion of reaction aqueous sodium bicarbonate solution is added and extracted in ethyl acetate (4×25 mL) from the aqueous layer and concentrated in vacuo afforded 2-methyl 4H-benzo[d][1,3]oxazin-4-one compound ( 28) as pure product. To a stirred solution of 4-((4-tertbutylphenyl)ethynyl)-2-methylbenzenamine (26b, 263 mg, 1 mmol) with 2-methyl-4H-benzo[d][1,3]oxazin-4-one (28, 161 mg, 1 mmol) in acetic acid and reflux for 8 h After completion of the reaction as indicated by TLC. then the reaction mixture was quenched with NaHCO3 and extracted in ethyl acetate (4×25 mL) from the ice cold aqueous layer and dried over anhydrous Na2SO4 afforded 3-(4-((4-tert-butylphenyl)ethynyl)-2-methylphenyl)-2-methylquinazolin-4(3H)-one (29b). Reaction of 3-(4-((4-tert-butylphenyl)ethynyl)-2-methylphenyl)-2-methylquinazolin-4(3H)-one (29b, 406 mg, 1 mmol) with 2,4-dihydroxybenzaldehyde (30d, 138 mg, 1 mmol) was taken in acetic acid Then the resulting mixture was stirred under reflux conditions for 8 h and then the reaction mixture was quenched with NaHCO3 and extracted in ethyl acetate (4×25 mL) from the ice cold aqueous layer and dried over anhydrous Na2SO4.The resulting product ( 5d) was purified by column chromatography employing EtOAc/Hexane as an eluent.

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.

Related Products of 1133123-02-0, 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 1133123-02-0 as follows.

A mixture of Intermediate 177c (crude boronic ester, 60 mg, 0.107 mmol) and 4- bromo-2-iodobenzoic acid (35.0 mg, 0.107 mmol) in NMP/H20 (1:1, 1 mL) was treated with K2C03 (32.6 mg, 0.236 mmol) followed by Pd2(dba)3 (9.80 mg, 10.71 muiotaetaomicron). The resulting mixture was degassed with N2 for 2 min before the reaction vessel was sealed and irradiated in a microwave reactor at 120 C for 15 min. The mixture was cooled and filtered through celite and purified via preparative HPLC (Column: Phenomenex AXIA Luna 100 x 30mm 5u s; Mobile Phase A: 10:90 ACN: H20 with 10 mM TFA; Mobile Phase B: 90: 10 ACN: H20 with 10 mM TFA; Gradient: 0-100% B over 10 minutes, then a 2-minute hold at 100% B; Flow: 40 mL/min.) to afford the title compound (Intermediate 195a, 17 mg, 0.037 mmol, 34.5 % yield). LC-MS (Method A5): 2.27 min, [M + H]+=465.1 and 467.1. 1H NMR (500 MHz, CDCl3) delta 7.91 (br d, 7=8.0 Hz, IH), 7.76 (br s, IH), 7.65 (br d, 7=7.7 Hz, IH), 7.44 (br s, 2H), 5.84 (br s, 2H), 3.26 (br s, 2H), 2.72 – 2.54 (m, 6H), 1.38 (br s, 3H).

According to the analysis of related databases, 1133123-02-0, the application of this compound in the production field has become more and more popular.

Synthetic Route of 6828-35-9, 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. 6828-35-9 name is 5-Chloro-2-iodoaniline, 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.

5-Chloro-2-((trimethylsilyl)ethynyl)aniline To a solution of 5-chloro-2-iodoaniline (1.50 g, 5.92 mmol) and ethynyltrimethylsilane (1.25 ml, 8.88 mmol) in Et3N (20 ml) was added CuI (5.6 mg, 0.030 mmol) and Pd(PPh3)2Cl2 (21 mg, 0.030 mmol) and the mixture was stirred at room temperature for 5 hours. Celite was added and the suspension was filtered, rinsed with EtOAc. The filtrate was concentrated in vacuo to yield Intermediate 1 as a yellow oil (1.32 g, 100%). 1H NMR (CHLOROFORM-d) delta: 7.20 (d, J=8.2 Hz, 1H), 6.69 (d, J=1.8 Hz, 1H), 6.63 (dd, J=8.2, 2.1 Hz, 1H), 4.30 (br. s., 2H), 0.27 (s, 9H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-Chloro-2-iodoaniline, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 461-17-6, name is 1,1,1-Trifluoro-4-iodobutane, 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 461-17-6, Recommanded Product: 461-17-6

Step 1. Preparation of tert-butvl fM-(4.4,4-trifluorobutvl)piperidin-3-vnmethvl)carbamate; O CH3T rcH3O CH3[122] To a mixture of tert-butyl (piperidin-3-ylmethyl)carbamate (0.30 g, 1.40 mmol) in anhydrousCH3CN (10 ml_) was added CsF-celite (0.53 g) followed by 1-iodo-4,4,4-trifluorobutane (0.40 g,1.68 mmol). The mixture was heated to reflux and stirred for 16 h. The mixture was diluted withEtOAc, filtered through a pad of Celite and then concentrated to dryness under reducedpressure. Water (40 ml_) was added, and the mixture was extracted with CH2CI2 (2 x 40 mL) andEtOAc (1 x 40 mL). The combined organic layers were dried over MgSO4, filtered, andconcentrated in vacuo. The white residue was taken up in CH2CI2 (with a minimal amount ofMeOH) and loaded onto a silica gel column. The mixture was then purified by silica gel flashchromatography (97% CH2CI2: 3% 2M NH3 in MeOH). This gave the product as a light yellow oil(0.31 mg, 68%). 1H NMR (300 MHz, CD3CN) 8 5.30 (br s, 1H), 2.86-2.90 (m, 2H), 2.66-2.73 (m,2H), 2.29-2.34 (m, 2H), 2.09-2.23 (m, 2H), 1.95-1.99 (m, 2H), 1.57-1.71 (m, 6H), 1.37 (s, 9H),0.83-0.99 (m, 1H); ES-MS m/z325.1 (MH+); HPLC RT (min) 1.76.

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, 1,1,1-Trifluoro-4-iodobutane, other downstream synthetic routes, hurry up and to see.

98-61-3, name is 4-Iodobenzenesulfonyl chloride, 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. Quality Control of 4-Iodobenzenesulfonyl chloride

To a solution of S-isoleucinol (0.50 g, 4.26 mmol), triethylamine (0.47 g, 4.68 mmol) and methylene chloride (10 mL) at 0C, was added a solution of 4-iodo benzenesulfonyl chloride (1.29 g, 4.26 mmol) in CH2C12 (5 mL). After 15 minutes the ice bath was removed and the reaction allowed to reach 25C. After 16 hours, the reaction was quenched by pouring into saturated sodium bicarbonate solution (22 mL) and additional methylene chloride (15 mL). The organic phase was separated and washed sequentially with IN HC1 solution (25 mL), distilled water and brine, dried over MGS04 and evaporated to give a crude solid that was recrystallized from ethyl acetate-hexane, mp 118-120C (1.07 g, 66%). MS (+APCI) 383.96 ([M+H] +) ; 283.81 ; 191.95. Anal. Calc’d for C12HL8LNO3S : C, 37.61 ; H, 4.73 ; N, 3.65 ; Found : C, 37. 55 ; H, 4. 61 ; N, 3. 61.

The synthetic route of 98-61-3 has been constantly updated, and we look forward to future research findings.