Month: April 2021

Some common heterocyclic compound, 25252-00-0, name is 2-Bromo-5-iodobenzoic acid, molecular formula is C7H4BrIO2, 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. HPLC of Formula: C7H4BrIO2

Preparation of 4-bromo-3-hydroxymethyl-1-iodo-benzene Oxalyl chloride (13.0 mL) is added to an ice-cold solution of 2-bromo-5-iodo-benzoic acid (49.5 g) in CH2Cl2 (200 mL). DMF (0.2 mL) is added and the solution is stirred at room temperature for 6 h. Then, the solution is concentrated under reduced pressure and the residue is dissolved in THF (100 mL). The resulting solution is cooled in an ice-bath and LiBH4 (3.4 g) is added in portions. The cooling bath is removed and the mixture is stirred at room temperature for 1 h. The reaction mixture is diluted with THF and treated with 0.1 M hydrochloric acid. Then, the organic layer is separated and the aqueous layer is extracted with ethyl acetate. The combined organic layers are dried (Na2SO4) and the solvent is evaporated under reduced pressure to give the crude product. Yield: 47.0 g (99% of theory)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 25252-00-0, 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. 25252-00-0, name is 2-Bromo-5-iodobenzoic acid, A new synthetic method of this compound is introduced below., Recommanded Product: 2-Bromo-5-iodobenzoic acid

2-Bromo-5-iodobenzoic acid (6.54 g, 20.0 mmol) was dissolved in DMF (70 mL). Potassium bicarbonate (2.2 g, 22.0 mmol) was added, followed by benzyl bromide (2.8 mL, 22.0 mmol). The mixture was stirred at rt under N2 for 12 h. The reaction mixture was poured into water and extracted with EtOAc. The combined organic solution was washed with brine, dried over MgSO4, and concentrated and dried to give 9.05 g of the benzyl ester.

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.

Adding a certain compound to certain chemical reactions, such as: 2974-94-9, name is 1-Iodo-4-phenoxybenzene, 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 2974-94-9, HPLC of Formula: C12H9IO

Example 356: 3-[1-(4-phenoxyphenyl)-3-(2-phenylethyl)-1H-indol-5-yl]propanoic acid 2-amino-2-(hydroxymethyl)propane-1,3-diol salt (1:1); Step 1; To a solution of the compound obtained at Example 142 (15.30 g) in toluene (76 ml) were added 4-iododiphenyl ether (28.18 g), copper(I) iodide (1.944 g), N,N’-dimethylethylenediamine (3.420 g) and tripotassium phosphate (21.186 g), and the mixture was heated and stirred at 92C for 5 hours. The reaction mixture was allowed to cool, then silica gel (15.3 g) was used to filter off the insolubles and the solvent was distilled off from the filtrate in vacuo to afford a crude product of ethyl 3-[1-(4-phenoxyphenyl)-3-(2-phenylethyl)-1H-indol-5-yl]propanoate.

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-Iodo-4-phenoxybenzene, other downstream synthetic routes, hurry up and to see.

These common heterocyclic compound, 101335-11-9, name is 2-Chloro-4-fluoro-1-iodobenzene, 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: 101335-11-9

To a solution of 2-chloro-4-fluoro-1 -iodo-benzene (9.0 g, 1 eq.) in DMF (46 ml.) was added cesium carbonate (22.8 g, 2 eq) then 4-chlorophenol (4.5 g, 1 eq.). The mixture was heated at 95 C for 16h. After cooling, an aq. solution of ammonium chloride (230ml_) was added, and extracted 3 times with diethylether. The organic phases were combined and washed successive- lywith an aq. solution of ammonium chloride (2x), aq. solution of NaOH (2%), water, then a saturated aq. solution of sodium chloride. The organic phase was dried and evaporated to give after purification on column chromatography on silica gel, 2-chloro-4-(4-chlorophenoxy)-1 -iodo- benzene as an oil (16,7 g, yield=47%).

The synthetic route of 2-Chloro-4-fluoro-1-iodobenzene has been constantly updated, and we look forward to future research findings.

Some common heterocyclic compound, 72373-82-1, name is 1-Chloro-2-fluoro-3-iodobenzene, molecular formula is C6H3ClFI, 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. Quality Control of 1-Chloro-2-fluoro-3-iodobenzene

(0112) A 500 mL flask was charged with 1-chloro-2-fluoro-3-iodobenzene (12.87 g, 65 mmol), [1,1′-biphenyl]-4-ylboronic acid (20 g, 78 mmol), potassium carbonate (8.98 g, 65 mmol), Pd(PPh3)4 (7.51 g, 6.5 mmol), toluene (280 ml), ethanol (140 ml) and water (140 ml). The resulting mixture was stirred, degassed and heated to 72C. for overnight. The reaction mixture was transferred into a separatory funnel, organic layer was separated, and aqueous layer was extracted with EtOAc. Combined organic layer was dried over Na2SO4, concentrated and the resulting residue was purified by column chromatography (EtOAc/heptane) to obtain 16.8 g (91% yield) of 3-chloro-2-fluoro-1,1′:4′,1”-terphenyl .

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 72373-82-1, its application will become more common.

Application of 19094-56-5, The chemical industry reduces the impact on the environment during synthesis 19094-56-5, name is 2-Chloro-5-iodobenzoic acid, I believe this compound will play a more active role in future production and life.

Equipped with a thermometer, constant pressure dropping funnel, drying tube 1000mL flask was added three DCM200mL, VIII (70.62g, 250mmol) ,was added 1 ml of DMF and, at room temperature was slowly added dropwise oxalyl chloride (23.4mL g, 275mmol), was added dropwise after the completion of 20 incubated 2h.After adding concentrated to remove the DCM, oxalyl chloride 200mL DCM dissolved chloride.Equipped with a thermometer, constant pressure dropping funnel, 1000mL three 26mL flask with a drying tube was added fluorobenzene, DCM200mL the system temperature was dropped to -5 deg.] C, graded added to the system aluminum trichloride (36.67g, 275mmol) , dropped acid chloride prepared raw reaction incubated 6h completed.System 40mL conc HCl + 400mL poured into ice water to quench the reaction, the DCM. The combined organic phases were washed until neutral sodium bicarbonate, once with saturated brine separation was washed with water, dried, and concentrated to give VII84.23g, yield 93.4%.

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, 2-Chloro-5-iodobenzoic acid, other downstream synthetic routes, hurry up and to see.

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. 628-77-3, name is 1,5-Diiodopentane, A new synthetic method of this compound is introduced below., COA of Formula: C5H10I2

Step 1: preparation of tert-butyl (trans-4-(piperidin-1-yl)cyclohexyl)carbamate Tert-butyl (trans-4-aminocyclohexyl)carbamate (214 mg, 1 mmol) and 1,5-diiodopentane (324 mg, 1 mmol) were dissolved in acetonitrile (5 mL). The reaction liquid was added with potassium carbonate (414 mg, 3 mmol), and reacted at 70 C for 2 hours. The reaction liquid was concentrated to dryness, dissolved in ethyl acetate (10 mL), washed with saturated brine, and the organic phase was dried over anhydrous sodium sulfate and concentrated under reduced pressure to give 250 mg of a pale yellow solid. Yield: 88.6%. MS (ESI, m/z): [M+H]+: 283.3.

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.

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., category: iodides-buliding-blocks

Into a 100-mL round-bottom flask was placed ACN (100 mL), 4-fluoro-2-methoxyphenol (5 g, 35.18 mmol, 1.00 equiv.), 1-chloro-3-iodopropane (14.4 g, 70.44 mmol, 2.00 equiv), and potassium carbonate (14.6 g, 105.64 mmol, 3.00 equiv). The resulting solution was stirred for 4 h at 80 C. The solids were filtered out. The resulting mixture was concentrated under vacuum. This resulted in 7.7 g (100%) of the title compound as a yellow oil. Analytical Data: LC-MS: (ES, m/z): RT = 1.365 mi m/z = 219 [M+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.

3819-88-3, name is 1-Fluoro-3-iodo-5-nitrobenzene, 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

Example 1 Step 1. To a solution of 1.0 eq IA in dry DMF (0.37 M) was added Zn(CN)2 (0.92 eq) and Pd(PPlIa)4 (0.058 eq). The reaction mixture was purged with nitrogen and heated to 800C overnight. An additional 0.023 eq of Pd(PPh3)4 was then added and the reaction was heated for another 6 hrs. The reaction mixture was then cooled to RT, diluted with 15 volumes of EtOAc (based on IA) and the organic layer was washed 3 times with water and once with brine. The organic layer was dried over sodium sulfate, filtered and concentrated. Purification by chromatography over silica gel using 10% E_2theta/hexane as the eluant provided IB as a solid (90%).

The synthetic route of 3819-88-3 has been constantly updated, and we look forward to future research findings.

Electric Literature of 6940-76-7, 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. 6940-76-7 name is 1-Chloro-3-iodopropane, 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.

1-(3-Chloropropyl)-3,4-dihydro-1H-quinolin-2-one (85LM31) A 50 mL flask was charged with 3,4-dihydro-1H-quinolin-2-one (2.00 g, 13.6 mmol) and sodium hydride (60% in oil, 0.712 g, 16.3 mmol) in DMF (50 mL, dry) and stirred at 0 C. for 1 h, followed by addition of 1-chloro-3-iodo-propane (2.77 g, 13.6 mmol) and stirring at rt for 20 h. The reaction mixture was quenched with water (10 mL), and the product was extracted into EtOEt (3*25 mL). The combined organic layers were dried (Na2SO4), evaporated and purified by flash CC (SiO2; EtOAc/heptane 1:4) to give the crude title compound (85LM31) (2.25 g). 1H NMR (CDCl3) delta 7.29-7.22 (m, 1H), 7.17 (d, J=7.4 Hz, 1H), 7.08-6.98 (m, 2H), 4.10 (t, J=7.3 Hz, CH2), 3.62 (t, J=5.9 Hz, CH2), 2.88 (t, J=7.3 Hz, CH2), 2.63 (t, J=7.3 Hz, CH2), 2.19-2.10 (m, 2H); 13C NMR (CDCl3) delta 170.5, 140.0, 128.2, 127.8, 126.3, 123.2, 115.0, 43.3, 40.2, 32.2, 30.5, 26.0.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Chloro-3-iodopropane, and friends who are interested can also refer to it.