Tag: M.W=200-300

Adding a certain compound to certain chemical reactions, such as: 20776-54-9, name is 2-Amino-4-iodobenzoic acid, 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 20776-54-9, Computed Properties of C7H6INO2

Embodiment 19 2-amino-4-((4,4-dimethylthiochroman-6-yl)ethynyl)benzoic acid 6-Ethynyl-4,4-dimethylbenzothiopyran (405.6mg, 2mmol) and 2-amino-4-iodobenzoic acid (263mg, 1mmol) were added to a flask, followed by addition of Pd(PPh3)2Cl2 (42mg, 0.06mmol) and CuI (23mg, 0.12mmol). After the flask was purged with argon for 3 times to remove oxygen, 10mL dry DMF and 0.2mL dry Et3N were added via syringe. Then the reaction was continued at 75C for 12 h and monitored by TLC. After completion of the reaction, the reaction solution was cooled to room temperature and the reaction was quenched with saturated ammonium chloride solution. The mixture was diluted with ethyl acetate, washed with saturated ammonium chloride solution and saturated sodium chloride solution. The organic phase was dried over anhydrous sodium sulfate, filtered, concentrated and purified by flash column chromatography (PE:EtOAc = 5:1) to give WYC-212 (286mg, 85%). 1H NMR (500 MHz, CDCl3) delta 7.88 (d, J = 8.3 Hz, 1H), 7.52 (d, J = 1.7 Hz, 1H), 7.18 (dd, J = 8.1, 1.8 Hz, 1H), 7.06 (d, J = 8.1 Hz, 1H), 6.84 (d, J = 1.3 Hz, 1H), 6.81 (dd, J = 8.3, 1.5 Hz, 1H), 3.08 – 3.02 (m, 3H), 1.99 – 1.94 (m, 2H), 1.35 (s, 6H); 13C NMR (126 MHz, CDCl3) delta 165.25, 165.23, 163.21, 161.20, 142.29, 134.42, 133.26, 133.25, 131.70, 131.64, 129.97, 129.27, 126.75, 125.15, 125.12, 117.73, 117.05, 116.92, 116.66, 116.47, 98.04, 98.02, 81.71, 61.62, 37.29, 33.13, 30.09, 23.38, 14.42. ESI(+)-MS: 338.3 [M+1]+.

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-Amino-4-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. 3930-83-4, name is 2-Iodobenzamide, A new synthetic method of this compound is introduced below., Formula: C7H6INO

General procedure: To a 25 mL Schlenk tube containing a solution of 2 in 2 mL of THF was added amide (1.0 mmol) and (EtO)3SiH (0.50 g, 3.0 mmol). The reaction mixture was stirred at 60 C until there was no amide left (monitored by TLC and GC-MS). The product was purified according to literature procedures by Beller

The synthetic route of 3930-83-4 has been constantly updated, and we look forward to future research findings.

Application of 90347-66-3, 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. 90347-66-3 name is Methyl 3-iodo-4-methylbenzoate, 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.

To a solution of 3-IODO-4-METHYL-BENZOIC acid methyl ester (13.50 g, 48.92 MMOL) in THF (260 mL) was added 2 M solution of ISOPROPYLMAGNESIUM chloride in THF (24.5 mL, 49.00 MMOL) AT-50C. After the reaction mixture was stirred at the same temperature for 30 min, compound 440 (13.39 G, 40.70 MMOL) was added. The solution was warmed up to room temperature and stirred at the same temperature for 2 h. The reaction was then quenched with saturated aqueous solution of NH4CI. The aqueous phase was extracted twice with diethyl ether. The combined organic phases were dried over MGS04 and concentrated in vacuo. The crude material was taken up in ethanol and heated for reflux. The obtained solution was cooled down to room temperature. The crystals were filtered off and dried

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl 3-iodo-4-methylbenzoate, and friends who are interested can also refer to it.

Electric Literature of 5876-51-7, These common heterocyclic compound, 5876-51-7, name is 5-Iodobenzo[d][1,3]dioxole, 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.

General procedure: A suspension of aryl halide (1.0 mmol), K2CO3 (2.0 mmol), Fe3O4SiO2-EDTA-Pd (0.008 g, 0.4 mol%) in H2O/DMF [2/1 (v/v)] (3 mL) was mixed in a reaction flask and n-butylacrylate or styrene (1.2 mmol) was added. The reaction mixture was stirred at 100 C for an appropriate time. After completion of the reaction (monitored by TLC), it was cold at room temperature, diluted with ethyl acetate (10 mL) and then the catalyst was separated from the solution by an external magnetic field. The organic phase was separated and dried over MgSO4 and the solvent was then removed under reduced pressure. Pure products were obtained after isolation of the residue by column chromatography on silica (hexane/ethyl acetate).

Statistics shows that 5-Iodobenzo[d][1,3]dioxole is playing an increasingly important role. we look forward to future research findings about 5876-51-7.

Electric Literature of 58313-23-8, A common heterocyclic compound, 58313-23-8, name is Ethyl-3-iodobenzoate, molecular formula is C9H9IO2, 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.

To a solution of ethyl 3-iodobenzoate (13.16 g, 47.70 mmol) in THF at -30 to -40 0C isopropylmagnesium chloride (23.8 mL of a 2M solution, 47.70 mmol) was added dropwise. The resulting mixture was stirred for one hour before 5- chloro-2-methylbenzaldehyde (7.0 g, 45.3 mmol) was added. The reaction mixture was stirred at -30 0C for 30 min, then warmed to room temperature and stirred for an additional 10 min. Aqueous NH4Cl and EtOAc were added and the layers separated. The organic layer was then washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The crude material was purified using silica gel chromatography to afford 10.2 g of ethyl 3-[(5-chloro-2- methylphenyl)(hydroxy)methyl]benzoate (70% yield).

The synthetic route of 58313-23-8 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 58313-23-8, A common heterocyclic compound, 58313-23-8, name is Ethyl-3-iodobenzoate, molecular formula is C9H9IO2, 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.

Ethyl 3-iodobenzoate (939mg, 3.40mmol) was dissolved in DMF (2mL) and a solution of 3-cyanophenylboronic acid (500mg, 3.40mmol) in DMF (5mL) was added. A solution of Pd(OAc)2 (15mg, 0.068mmol) and Na2C03 (858mg, 10.2mmol) in water (2mL) was added and the reaction mixture was heated at 110C for 2d. The reaction mixture was concentrated in vacuo and partitioned between DCM (150mL) and water (50mL). The aqueous fraction was extracted with DCM (50mL) and the combined organic fractions were dried (MgSC^) and concentrated in vacuo. The residue was purified by column chromatography to give the title compound (767mg, 90%) as a pale yellow liquid. LCMS: ES+ 252.1 [MH]+.

The synthetic route of 58313-23-8 has been constantly updated, and we look forward to future research findings.

Electric Literature of 31599-61-8,Some common heterocyclic compound, 31599-61-8, name is 4-Iodo-1,2-dimethylbenzene, molecular formula is C8H9I, 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: 3,4-Dimethyl iodobenzene (0.10 mol) was dissolved in xylene (200 mL), and bistriphenylphosphine palladium dichloride was added.(0.0005 mol) and tert-butyl potassium (0.20 mol), after stirring, 3-aminopentane (0.11 mol) was added, the reaction temperature was adjusted to 90 C, and the reaction was carried out for 6 hr. After the reaction, the mixture was cooled to room temperature, and filtered. 100 ml of 5% aqueous citric acid solution, 100 ml of saturated sodium carbonate solution,Wash with 100 ml of saturated brine and dry over anhydrous sodium sulfate.The mixture was concentrated under reduced pressure until the liquid surface was not foamed to afford 18.4 g of an oily product. The product yield was 96.3% based on 3,4-dimethyl iodobenzene, and the purity was determined by HPLC to be 96.8 %.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-Iodo-1,2-dimethylbenzene, its application will become more common.

These common heterocyclic compound, 1829-28-3, name is Ethyl 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: C9H9IO2

In a test tube equipped with a stirring bar and a septum rubber,Under argon flow, bis (trifluoromethyl) zinc (DMPU) 2 complex (92 mg, 0.2 mmol),After adding copper (I) chloride (1.9 mg, 0.01 mmol), DMPU (0.2 ml) and ethyl 2-iodobenzoate (0.1 mmol, 16.6 mul)Replace septum rubber with screw cap,The reaction was carried out at 50 ° C. for 24 hours.After completion of the reaction,After cooling,As a result of quantification by 19 F-NMR using benzotrifluoride using the reaction solution as an internal standard substance,The yield of the objective ethyl 2- (trifluoromethyl) benzoate was 82percent.

The synthetic route of Ethyl 2-iodobenzoate has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 25309-64-2, name is 1-Ethyl-4-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 25309-64-2, Recommanded Product: 1-Ethyl-4-iodobenzene

Step-1: Synthesis of tert-butyl (Z)-(2-(4-(2-(4-ethylphenyl)-l-(4-hydroxyphenyl)but-l-en-l- yl)phenoxy )ethyl)carbamate To a stirred solution of tert-butyl (E)-(2-(4-(l-(4-hydroxyphenyl)-2-(4,4,5,5-tetramethyl- l ,3,2-dioxaborolan-2-yl)but-l-en-l-yl)phenoxy)ethyl)carbamate (1.3 g, 2.55 mmol, Example- 46, Step-1) in 2-methyl THF (15 mL), l-iodo-4-ethylbenzene (0.651 mg, 2.8 mmol), 4M aqueous KOH (2 mL) and Pd(PPh3)2Cl2 (89 mg, 0.127 mmol) were added and the mixture was degassed with nitrogen for 15 min and heated at 85 C for 3 h. Upon completion, the reaction mixture was diluted with EtOAc. The organic layer was washed with water followed by brine, dried over anhydrous sodium sulphate, filtered and concentrated under reduced pressure. The crude product was purified by silica gel chromatography (2:8 EtOAc in n- hexane) to give title compound (0.5 g, 40%).

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-Ethyl-4-iodobenzene, other downstream synthetic routes, hurry up and to see.

Electric Literature of 19099-54-8, These common heterocyclic compound, 19099-54-8, name is 1-Iodo-2-isopropylbenzene, 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.

0.3 mmol of sodium carbonate, 0.1 mmol of 1,2-bis(4-methoxyphenyl)acetylene, 0.005 mmol of palladium acetate, 0.005 mmol of bis(2-diphenylphosphinophenyl)ether, and pinacol borate 0.15mmol, 0.15mmol of 2-isopropyliodobenzene and 1mL of N,N-dimethylformamide were added to a 15mL reaction tube, and the nitrogen was repeatedly filled 10 times, placed in an oil bath at 120 C for 24 hours; cooling The reaction solution was diluted with ethyl acetate to room temperature.Wash three times with water, dry the organic phase with anhydrous Na2SO4, and filter.concentrate,Purification by thin layer chromatography gave 24.7 mg of the desired product.The yield was 51%. The nuclear magnetic and high resolution mass spectra of this compound are characterized as follows:

The synthetic route of 19099-54-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Huaqiao University; Cheng Guolin; Lv Weiwei; (10 pag.)CN109879899; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com