Month: May 2021

Related Products of 447464-03-1, A common heterocyclic compound, 447464-03-1, name is 2-Fluoro-3-iodobenzoic acid, molecular formula is C7H4FIO2, 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.

[0459] A solution of Example 73a (3.0 g, 11.2 mmol) and KBr03 (3.7 g, 22.0 mmol) in 15 mL of cone. H2S04. The reaction mixture was stirred for 2 h at 90C; LC-MS (BD01052-127) analysis showed Example 73a was consumed; the mixture was poured into 250 mL water and stirred for 10 min. The mixture was extracted with EA (250 mL * 3). The combined organic phase was dried over Na2S04, filtrated and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel chromatography to give the desired product (Example 73b, 3.5 g, yield: 65%) as a yellow solid.LCMS [M+l]+ = 344.0

The synthetic route of 447464-03-1 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 52914-23-5, 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. 52914-23-5 name is 2-(4-Iodophenyl)ethanol, 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 solution of N,N(-bis(tert-butoxycarbonyl)-S-methylisothiourea (937 mg, 3.2 mmol), triphenylphosphine (5.0 g, 18 mmol) and 2-[(4-iodophenyl)ethyl]alcohol (1a, 800 mg, 3.2 mmol) were stirred in anhydrous THF (16 mL) at room temperature under nitrogen atmosphere. DIAD (3.8 ml, 18 mmol) was slowly added to reaction mixture and reaction was stirred at room temperature for 24 h. The reaction mixture was filtered through a Celite pad with washing CH2Cl2 and the solvent was removed under reduced pressure. The residue was purified by flash column chromatography (silica gel, 5% ethyl acetate in hexane) to afford the product 2 (1.1 g, 66%) as a colorless oil; 1H NMR (400 MHz, CDCl3) (7.61 (d, J = 8.4 Hz, 2H), 6.98 (d, J = 8.0 Hz, 2H), 3.72-3.64 (m, 2H), 2.96-2.88 (m, 2H), 2.37 (s, 3H), 1.51 (s, 9H), 1.48 (s, 9H); 13C NMR (100 MHz, CDCl3) (162.7, 158.0, 151.8, 138.2, 137.7, 131.1, 91.8, 82.7, 82.1, 50.1, 34.9, 28.2, 28.1, 15.8; HRMS (FAB) calcd for C20H30IN2O4S (M+) 521.0971, found 521.0966.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-(4-Iodophenyl)ethanol, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 19393-94-3, name is 2,4-Dibromo-1-iodobenzene, 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 19393-94-3, COA of Formula: C6H3Br2I

Into a 100ml two-necked flask feed 2, 4-dibromo-1-iodobenzene (3.6g), trimethylsilylacetylene (1. 1g), CuI (O.11g), Pd(PPh3)2C12 (0.21g) molar ratio is based on 1:1.1 :0.06:0.03, solvent selection as 50ml anhydrous tetrahydrofuran, anhydrous anaerobic conditions are controlled at 0 C, stir for 30 minutes, distillation under reduced pressure and then obtained 3.16g of ((2,4-dibromophenyl) ethynyl) trimethylsilane, yield is 95%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2,4-Dibromo-1-iodobenzene, and friends who are interested can also refer to it.

Related Products of 1000577-94-5, A common heterocyclic compound, 1000577-94-5, name is 3-Bromo-4-iodobenzonitrile, molecular formula is C7H3BrIN, 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.

In a nitrogen stream, in a 50 mL Schlenk tube,3.52 g (11.43 mmol) of 3-bromo-4-iodobenzonitrile, 6.35 g (28.58 mmol) of 9-phenanthreneboronic acid,51 mg (0.23 mmol),218 mg (0.46 mmol) of 2-dicyclohexylphosphino-2 ‘, 4′, 6’-triisopropylbiphenyl (Xphos), 15 mL of tetrahydrofuran,And 15 mL of 2 M potassium carbonate aqueous solution were added, and the mixture was stirred at 75 C. for 15 hours. After cooling to room temperature, methanol 100 mL was added and stirred, and the precipitated solid was collected by filtration and washed with pure water and methanol.By recrystallizing (chloroform / methanol) the residue,1.62 g (3.56 mmol) of a colorless powder of 9- [4-cyano-2- (9-phenanthryl) -phenyl] – phenanthrene was isolated (yield 31%, HPLC purity 98.4%).

The synthetic route of 1000577-94-5 has been constantly updated, and we look forward to future research findings.

Reference of 141738-80-9,Some common heterocyclic compound, 141738-80-9, name is 3-Chloro-4-iodobenzotrifluoride, molecular formula is C7H3ClF3I, 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.

General procedure: For a typical reaction, a Vapourtec 2R+ Series was used as the platform with a Vapourtec Gas/Liquid Membrane Reactor to load the carbon monoxide. The HPLC pump were both set at 0.125 mL/min, temperature of the reactor at 110 C, pressure of CO at 15 bar with a back pressure regulator of 250 psi (17.24 bar). The system was left running for 2 h to reach steady state after which time the flow streams were switched to pass from the loops where the substrates and catalysts were loaded. The first loop (5 mL) was filled with a solution of palladium acetate (20 mg, 0.08 mmol), triphenylphosphine (48 mg, 0.168 mmol) in 6 mL of 1,4-dioxane while the second loop (5 mL) was filled with a solution made from the ortho-substituted iodoarene substrate (1.68 mmol), triethylamine (0.272 g, 0.374 mL, 2.69 mmol) and water (0.505 g, 28 mmol) in 5.8 mL of 1,4-dioxane. An Omnifit column filled with 1.71 cm3 (r = 0.33 cm, h = 5.00 cm) of cotton was positioned just before the back pressure regulator to trap any particulate matter formed to avoid blocking of the back pressure regulator. After the substrates were passed through the system, the outlet of the flow stream was directed into a receptacle where the excess carbon monoxide gas was vented off in the fume cupboard. The reaction mixture was then evaporated to dryness, ethyl acetate (25 mL) and sodium carbonate solution (2 M, 10 mL) were added and transferred to a separating funnel. After collecting the aqueous layer, the organic layer was extracted with sodium carbonate solution (2 M, 2 × 10 mL). The combined aqueous layers were acidified by the addition of 2 M HCl solution which was then extracted with ethyl acetate (3 x 25 mL). The organic layer was dried over sodium sulfate, and the solvent evaporated under vacuum to give the crude product as a solid. The crude product was then recrystallised from the appropriate solvent.

The synthetic route of 141738-80-9 has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 74128-84-0, name is 2-Bromo-1-iodo-3-methoxybenzene, 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. Quality Control of 2-Bromo-1-iodo-3-methoxybenzene

Under a nitrogen atmosphere, 31.3 g of 2-bromo-1-iodo-3-methoxybenzene,Phenyl dibenzo [b, d] furan-2-amine (26.0 g), A flask containing sodium-tert-butoxide (14.6 g) and toluene (200 ml) was heated to 90 C and bis [(tri-tertiary-butyl) phosphine] palladium (2.0 g) was added thereto. And refluxed under nitrogen for 24 hours.After cooling to room temperature, the mixture was filtered, and the solvent was distilled off under reduced pressure. The resulting solid was washed with acetonitrile to obtain 22.2 g of compound synthesis intermediate E

The synthetic route of 2-Bromo-1-iodo-3-methoxybenzene has been constantly updated, and we look forward to future research findings.

Electric Literature of 1208075-44-8, 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. 1208075-44-8, name is Ethyl 2-bromo-5-iodobenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a 20 mL vial with a stir bar was added aryl halide 1 (2.00 mmol), Pd(dba)2 (28.8 mg, 2.5 mol %), Xantphos (28.9 mg, 2.5 mol %). The vial was sealed with a Teflon-lined cap and THF (6.0 mL) was added. The mixture was vacuumed and backfilled with nitrogen (3×). A solution of ethyl 2-bromozincacetate (2a) in THF (0.40 M, 6.0 mL, 1.2 equiv) filtered through a Target Nylon 0.45 mum filter (1.25-inch OD) was syringed in and the reaction mixture was then heated to 65 C and monitored by HPLC. Upon reaction completion based on HPLC analysis (?95% conversion unless the reaction was stalled), the mixture was cooled to room temperature and quenched with 1 M aq HCl (5.0 mL), followed by addition of brine (5.0 mL). The organic layer was separated and concentrated in vacuum. The residue was purified by silica gel column chromatography using gradient EtOAc in hexanes.

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 2-bromo-5-iodobenzoate, 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. 136618-42-3, name is Benzyl 4-iodobenzoate, A new synthetic method of this compound is introduced below., SDS of cas: 136618-42-3

Intermediate 8: Phenylmethyl 4-(4-amJno-6-methyl-1 H-indazol-1-yl)benzoate; 6-Methyl-1 /-/-indazol-4-amine (5.48g, 37.3mmol), copper (I) iodide (71 mg, 0.37mmol), frans-1 ,2-cyclohexanediamine (420mg, 0.37mmol) and tripotassium phosphate (16.6g, 78.3mmol) were added to a solution of phenylmethyl 4-iodobenzoate (12.61g, 37.3mmol) in 1 ,4-dioxane (2OmL). More 1 ,4-dioxane (3OmL) was added and the mixture heated under reflux for 3 hours 15 min and then allowed to gradually cool to room temperature and partitioned between water and ethyl acetate. The aqueous phase was extracted once more with ethyl acetate and the combined organic extracts were washed with brine and dried and evaporated to give a brown solid (13.58g). This crude product was combined with material (0.66g) from a similar reaction and purified by column chromatography on silica gel (Merck 7734, 50OmL) eluting initially with 10% and finally with 20% ethyl acetate in dichloromethane. Evaporation of product containing fractions gave a brown-yellow solid (5.12g) which was dissolved in ethyl acetate (4OmL) at 60 and warm cyclohexane (7OmL) was added. The mixture was then cooled in ice and the precipitate was collected by filtration, washed with cyclohexane:ethyl acetate (4:1 , 4OmL) and dried to give the title compound as a beige solid (4.29g). LCMS (System A): tRET = 3.77 min; MNH4+ = 358

The synthetic route of 136618-42-3 has been constantly updated, and we look forward to future research findings.

Related Products of 19393-94-3,Some common heterocyclic compound, 19393-94-3, name is 2,4-Dibromo-1-iodobenzene, molecular formula is C6H3Br2I, 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.

Add 30.0 g of intermediate 1-1,500 ml of N,N-dimethylformamide to a 1 L three-necked flask, and replace the nitrogen gas. Then added 75.3 g of intermediate 1-2, 57.5 g of potassium carbonate, 1.2 g of bis(2-diphenylphosphinophenyl) ether, 2.4 g of palladium acetate; The reaction solution was heated to 150 C, and the reaction was stirred for 24 hours. The reaction was stopped after TLC was monitored to complete the reaction. After the reaction solution was cooled to room temperature, it was poured into 1.5 L of water to precipitate a solid. After washing with water to neutral, the crude product was passed through a column, and toluene was recrystallized to give 42.4 g of intermediate 1 in a yield of 68.5%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,4-Dibromo-1-iodobenzene, 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. 83027-73-0, name is 5-Bromo-1-chloro-3-fluoro-2-iodobenzene, A new synthetic method of this compound is introduced below., name: 5-Bromo-1-chloro-3-fluoro-2-iodobenzene

Dry methanol (160 mL) was cooled to 10 C and potassium hydroxide (14.9 g) was added portion wise over 25 minutes. Once dissolved, this solution was added over 15 minutes to a refluxing solution of 5-bromo-1-chloro-3-fluoro-2-iodo-benzene (CAS 83027-73-0, 40.0 g) in dry methanol (320 mL). After 46 hours refluxing the reaction mixture was concentrated and partitioned between water (500 mL) and ethyl acetate (500 mL). The aqueous phase was extracted with further ethyl acetate (2 x 200 mL). The combined organic layers were washed with brine (400 mL), dried over magnesium sulfate, concentrated and purified by chromatography on silica eluting with ethyl acetate in iso-hexane to give 5-bromo-1-chloro-2- iodo-3-methoxy-benzene (37.767 g) as a pale pink solid 1H NMR (500 MHz, CDCI3) 7.28 (d, 1 H), 6.82 (d, 1 H), 3.90 (s, 3H).

The synthetic route of 83027-73-0 has been constantly updated, and we look forward to future research findings.