Iodides-buliding-blocks

Adding a certain compound to certain chemical reactions, such as: 33994-44-4, name is Methyl 3-(4-Iodophenyl)propanoate, 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 33994-44-4, name: Methyl 3-(4-Iodophenyl)propanoate

A 500 ml three-neck flask is charged with 14.0 g of 4-(2-thienyl)acetoanilide, 22.4 g of methyl 4-iodophenylpropionate, 13.4 g of potassium carbonate, 0.8 g of copper sulfate pentahydrate and 40 ml of o-dichlorobenzene, and the mixture is stirred under heating at 200 C. for 15 hours in a nitrogen stream. After this reaction, 100 ml of ethylene glycol and 5.4 g of potassium hydroxide are added to the reaction mixture, which is then refluxed under heating for 3 hours in a nitrogen stream, then cooled to ambient temperature, poured into 300 ml of distilled water and neutralized by hydrochloric acid to thereby precipitate crystals. The crystals are filtered, sufficiently washed with water and then transferred to a 1 L flask. To the crystals is added 500 ml of toluene, followed by refluxing under heating to remove water by azeotropic distillation. Then, 100 ml of methanol and 1 ml of concentrated sulfuric acid are added thereto, and the resulting mixture is refluxed under heating for 2 hours in a nitrogen stream. After the reaction, the reaction solution is dissolved in distilled water and extracted with toluene. The organic phase is sufficiently washed with distilled water. Next, the organic phase is dried by sodium sulfate anhydride, a solvent is evaporated off under reduced pressure and the residue is recrystallized from an ethyl acetate-hexane mixed solution to thereby obtain 15.1 g of diarylamine. A 100 ml flask is charged with 5.5 g of the thus-obtained diarylamine, 3.2 g of 4,4-diiodobiphenyl, 2.2 g of potassium carbonate, 0.2 g of copper sulfate pentahydrate and 10 ml of o-dichlorobenzene, and the mixture is refluxed under heating for 9.5 hours in a nitrogen stream. After the reaction is completed, the reaction mixture is cooled to ambient temperature and dissolved in 100 ml of toluene, and unnecessary substances are removed by filtration. An obtained filtrate is purified by silica gel column chromatography using toluene, to thereby yield 6.2 g of a thiophene-containing compound (Exemplary Compound 7). A melting point of the resulting thiophene-containing compound is 110 to 112 C. The IR spectrum (obtained using a KBr tablet method) of the thiophene-containing compound is shown in FIG. 2. An 1H-NMR spectrum (in a CDCl3 solvent) of the thiophene-containing compound is shown in FIG. 3.

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, Methyl 3-(4-Iodophenyl)propanoate, other downstream synthetic routes, hurry up and to see.

Adding a certain compound to certain chemical reactions, such as: 199786-58-8, name is (5-Bromo-2-iodophenyl)methanol, 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 199786-58-8, Product Details of 199786-58-8

To a stirred mixture of alcohol 2-iodo-5-bromobenzyl alcohol (9.14 g, 29.2 mmol) in of CH3Cl (150 mL) under argon was added 1M PBr3 in CH2Cl2 (35.0 mL, 35.0 mmol). The reaction mixture was stirred at room temperature for 20 minutes and then poured into a mixture of ice and saturated NaHCO3 solution (300 mL). The pH was adjusted to basic by addition of solid NaHCO3. This aqueous layer was extracted with EtOAc (1×600 mL, 2×400 mL). The combined EtOAc extracts were washed with brine (1×100 mL). The organic layer was dried (MgSO4), filtered and concentrated in vacuo to give 2-iodo-5-bromobenzyl bromide (5.69 g, 52%). 1H NMR (CDCl3): delta=7.68 (d, 1H, J=8.80 Hz), 7.59 (s, 1H), 7.18 (d, 1H, J=8.80 Hz), 4.51 (s, 2H). HPLC: Rt=3.87 min.

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, (5-Bromo-2-iodophenyl)methanol, 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 573764-31-5 as follows. name: 4-Chloro-3-iodoaniline

General procedure: A mixture of compound 3 (5 mmol), phenylboronic acid (10 mmol), Pd(Ph3P)4 (0.1 mmol), Na2CO3 (10 mmol) in 1,4-dioxane/H2O (20 mL) was stirred at 110 °C for 24 h under Ar. The reaction mixture was filtered through celite. The filtrate was concentrated in vacuo and then extracted with EtOAc. The organic layer was evaporated to give a residue, which was purified by chromatography (petroleum ether/EtOAc, 10:1) to give pure product as a yellow liquid, yield 88percent.

According to the analysis of related databases, 573764-31-5, the application of this compound in the production field has become more and more popular.

Some common heterocyclic compound, 90347-66-3, name is Methyl 3-iodo-4-methylbenzoate, molecular formula is C9H9IO2, 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. Application In Synthesis of Methyl 3-iodo-4-methylbenzoate

A mixture of methyl 3-iodo-4-methylbenzoate (1.0 g, 3.6 mmol) and CuCN (389 mg, 4.3 mmol) in NMP (10 mL) is stirred at 200 oC for 1 hour with microwave irradiation.The mixture is diluted with EtOAc / toluene (10:1, 50 mL) to afford precipitate, which is separated by filtration through a pad of Celite. The filtrate is washed with water (30 mL x 3), brine (20 mL x 1), dried over sodium sulfate.The insoluble materials are separated by filtration and the filtrate is concentrated.The residue is purified by column chromatography on silica-gel eluting with n-hexane / EtOAc (7:1 to 6:1) to give 511 g (81% yield) of the title compound as a white solid. 1H-NMR (400 MHz, CDCl 3) delta8.27 (1H, d, J = 1.8 Hz), 8.13 (1H, dd, J = 8.6, 1.8 Hz), 7.42 (1H, d, J = 8.6 Hz), 3.94 (3H, s), 2.61 (3H, s).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 90347-66-3, its application will become more common.

Related Products of 624-75-9,Some common heterocyclic compound, 624-75-9, name is 2-Iodoacetonitrile, molecular formula is C2H2IN, 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.

Cyanomethyl)trimethylphosphonium iodide was prepared according to the general method described in Zaragoza, F., et al., J. Org. Chem.2001, 66, 2518-2521. In a 1 L round bottom flask, trimethylphosphine in toluene (100 mL, 100 mmol) was diluted with THF (50.0 mL) and toluene (50.0 mL), and cooled on an ice bath. The reaction mixture was stirred vigorously while iodoacetonitrile (7 mL, 16.7 g, 68.3 mmol) was added dropwise to produce a tan precipitate. The cooling bath was removed and the reaction mixture was stirred overnight at room temperature. The flask was placed in a sonicator to break up any clumped solids. The reaction mixture was stirred an additional 4 hours. The solids were collected by filtration and dried under vacuum to give (1380) (cyanomethyl)trimethylphosphonium iodide (16.6 g, 68.3 mmol, 68.3 % yield). 1H NMR (400 MHz, DMSO-d6) 4.03 (d, J=16.4 Hz, 2H), 2.05 (d, J=15.4 Hz, 9H).

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

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 627-31-6 as follows. Quality Control of 1,3-Diiodopropane(stabilized with Copper chip)

The beta- lactam carbonyl compound shown in the formula CH3CH2-COCH2CONH-C6H4Cl1.0mmol added 50 ml round-bottomed flask, and then sequentially adding K2CO32.4mmol, 0.10 mmol tetrabutylammonium chloride, ammonium acetate 1.1mmol, 1,3Diiodopropane 1.2mmol and 35mL of deionized water and mix well. The reaction was continued stirring at 20 10.0 hours, the reaction was stopped by filtration, dried and purified by recrystallization after give 6- (4-chloro-anilino) -5-propionyl-3,4-dihydropyran, products yield 96%.

According to the analysis of related databases, 627-31-6, the application of this compound in the production field has become more and more popular.

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.

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.

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.

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.