Month: April 2021

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.

199850-56-1, name is Methyl 2-amino-4-chloro-5-iodobenzoate, 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

Methyl 2-acetamido-4-chloro-5-iodobenzoate A mixture of methyl 2-amino-4-chloro-5-iodobenzoate (8.4 g, 0.027 mol), pyridine (6.4 g, 0.081 mol) in dichloromethane (250 mL) at 0 oC, acetyl chloride (2.5 g, 0.032 mol) was added. The mixture was stirred at RT for 16 h. The reaction mixture was washed with brine. The organic layer was dried over anhydrous Na2SO4, filtered and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel (ethyl acetate/petroleum ether = 1:5) to afford the desired product (7.6 g, 80% yield). ESI-MS m/z:353.9 [M + H]+.

The synthetic route of 199850-56-1 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 98-61-3, 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 98-61-3 as follows.

General procedure: To a solution of pyrrolidine (0.5 mL) and DIPEA (0.5 mL) in 5 mL THF was added dropwise at 0 C a solution of 4-iodobenzenesulfonyl chloride (300 mg, 1 mmol) in THF (2 mL). The mixture was stirred overnight, diluted with ethyl acetate, washed with 1 N HCl solution and water, concentrated, and dried under vacuum. 1-(4-iodobenzenesulfonyl)pyrrolidine (310 mg, 92%) was obtained.

According to the analysis of related databases, 98-61-3, the application of this compound in the production field has become more and more popular.

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 21304-38-1 as follows. Formula: C6H7IN2

A solution of 4-iodo-benzene-l,2-diamJne (0.46g, 1.96mmol), ethanedial [40% in water] (2.25mL), acetic acid (ImL) and ethanol (2OmL) were heated to 1000C for several hours and then cooled to room temperature. Water was added and the crude product was extracted with ethyl acetate. The product was purified via silica gel column chromatography with hexane: ethyl acetate (1:1) to give 0.323g (64%) of 6- iodo-quinoxaline. 1H NMR (400 MHz, CDCl3) S 8.77 (dd, 2H, J=2.0, 8.8Hz), 8.46 (d, IH, 2.0Hz), 7.96 (dd, IH, J=2.0, 8.8Hz), 7.75 (d, IH, J=8.8Hz).

According to the analysis of related databases, 21304-38-1, the application of this compound in the production field has become more and more popular.

Some common heterocyclic compound, 167479-01-8, name is tert-Butyl (3-iodopropyl)carbamate, molecular formula is C8H16INO2, 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. Computed Properties of C8H16INO2

Step B: Methyl 2-(5-(bis(tert-butoxycarbonyl amino -4-phenylpyrimidin-2-yl -5-((tert- butoxycarbonyl)amino)pentanoateTo a mixture of 2-((5-(bis-ter?-butoxycarbonyl)amino-4-phenylpyrimidin-2-yl)) acetate (300 mg, 0.676 mmol) and tert-butyl (3-iodopropyl) carbamate (231 mg, 0.812 mmol) in THF (6 mL) at 25 C was added potassium 2-methylpropan-2-olate (1.35 mL, 1.35 mmol). The resulting mixture was stirred at 25 C for 12 h then partitioned between water (30 mL) and EtOAc (30 mL x 3). The combined organic layers were dried over a2S04 and concentrated to give the title compound. MS: m/z = 601.4 (M + 1).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 167479-01-8, its application will become more common.

Adding a certain compound to certain chemical reactions, such as: 626-44-8, name is 1,3,5-Triiodobenzene, 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 626-44-8, Product Details of 626-44-8

Ethynyl-dC was synthesized following the procedure of Dodd et ah, Org. Biomol. Chem. (2010) 8:663-6665. Ethynyl-dC (0.2 g, 0.796 mmol) was then dissolved in DMF (10 mL) and maintained under nitrogen atmosphere. To this solution NEt (0.1.12 mL, 7.96 mmol), 1,3,5-triiodobenzene (1.11 g, 2.39 mmol), Pd(Ph P)4 (92 mg, 0.080 mmol) and Cul (31 mg, 0.16 mmol) were added sequentially with stirring under nitrogen. The reaction was continued at rt for 2 h and TLC (10percent MeOH in DCM) and LCMS (ES+) indicated complete disappearance of starting material. After removing the solvent under reduced pressure, the residue was chromatographed on silica gel column using 0 – 20percent MeOH gradient over DCM) to get pure product (0.324 g, 70percent). TLC:(10percent MeOH in DCM): Rf = 0.52. LCMS (ES+): (M+H) calculated mass: 579.14 and observed mass: 579.31. 1H-NMR (DMSO-d6): delta 8.82 (bs, 2H, 4-NH2), 8.38 (s, 1H, 6-H), 8.06 (t, 1H, Ar-H), 8.00 (d, 2H, Ar-H), 6.10 (t, 1H, l’-H), 5.22 (d, 1H, 2′-OH), 5.13 (t, 1H, 5′- OH), 4.22 (m, 1H, 4H), 3.80 (m, 1H, 3′-H), 3.63 – 3.68 (m, 1H, 5′-H), 3.55 – 3.61 (m, 1H, 5″-H), 2.15 – 2.22 (m, 1H, 2′-H), 1.98 – 2.04 (m, 1H, 2″-H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,3,5-Triiodobenzene, and friends who are interested can also refer to it.

Some common heterocyclic compound, 19230-28-5, name is 1,3-Dichloro-2-iodobenzene, molecular formula is C6H3Cl2I, 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: 19230-28-5

General procedure: To a stirred solution of complex 1 (10 mg, 0.0125 mmol) in a mixed solvent of n-heptane (1.5 mL) and water (1.5 mL) were added KCN (10.6 mg, 0.1625 mmol), ZnCl2 (11.1 mg, 0.0825 mmol), NaBH4 (0.5 mg, 0.0125 mmol), and iodobenzene (26 mg, 0.125 mmol). The reaction mixture was stirred at 100 C for 1 h under nitrogen atmosphere. After cooling the reaction mixture in an ice-bath, aliquots of the organic layer were transferred to a vial with a Pasteur pipette. Eluting the aliquots with diethyl ether on a short glass-column (0.7 × 15 cm) packed with alumina (ca. 1 cm) resulted in a clear yellowish solution which was analyzed with GC/MS.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 19230-28-5, its application will become more common.

Related Products of 260558-15-4, The chemical industry reduces the impact on the environment during synthesis 260558-15-4, name is 4-Bromo-2-iodo-1-methylbenzene, I believe this compound will play a more active role in future production and life.

To a solution of 2-methyl-5-bromo-iodobenzene (12 g, 40.4 mmol) in tetrahydrofuran (75 ml), cooled to -78 C., was added a solution of isopropylmagnesium chloride (4.6 g, 44.5 mmol) in tetrahydrofuran (22.2 ml) dropwise over 20 minutes. After stirring at -78 C. for 30 minutes, the mixture was warmed slowly to -20 C. and stirred for 1 hour. After cooling again to -78 C., trimethylborate (8.4 g, 80.8 mmol) was added dropwise. After warming to 0 C., the mixture was stirred for 2 hours, treated with 1 M hydrochloric acid (35 ml), and extracted with ethyl acetate (2*50 ml). The combined extracts were washed with water (50 ml), dried over sodium sulfate, and concentrated under reduced pressure. The residual solid was suspended in hexane (50 ml), filtered, washed with hexane (30 ml) and dried under reduced pressure to provide 2-methyl-5-bromo-phenylboronic acid (7.32 g, 84% yield) as a white solid. 1H NMR (DMSO-d6) delta 7.92 (s, 1H), 7.46 (d, J=8.1 Hz, 1H), 7.13 (d, J=8.1 Hz, 1H), 2.59 (s, 3H).

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, 4-Bromo-2-iodo-1-methylbenzene, other downstream synthetic routes, hurry up and to see.

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. 69113-59-3, name is 3-Iodobenzonitrile belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 69113-59-3

The title compound (39 mg, 67.3 %, yellow solid) was obtained from [4- (5-] tributylstannanyl-isoxazol-3-ylmethyl)-piperazine-1-carboxylic acid ethyl ester (106 mg, 0.2 mmol) and Pd (PPh3) [2C12] (0.2 mg) with 3-iodobenzonitrile (38.9 mg, 0.17 mmol) in dioxane [(LML)] at [110 C OVEMIGHT. LH-NMR] (CDC13) 8 (ppm): [8.] 07 (s, 2H), 8.02 (d, 1H), 7.73 (d, 1H), 7.62 (t, lH) 6.68 (s, [1H),] 4.14 (q, 2H), 3.68 (s, 2H), 3.51 (m, 4H), 2.51 (m, 4H) and 1. 26 (t, 3H).

The synthetic route of 69113-59-3 has been constantly updated, and we look forward to future research findings.

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 689291-89-2 as follows. Safety of 5-Bromo-2-iodobenzaldehyde

Intermediate 21; N-[(l£)-(5-bromo-2-iodophenyI)methylidene]-2-methyl-2- ropanamine; To a solution of 2-1, 4-Br benzaldehyde (2.0 g, 6.4 mmol) in anhydrous THF (10 mL) was added tert-butylamine (2.0 mL, 19.3 mmol) and the reaction stirred at room temperature under a nitrogen atmosphere for 4 days. The reaction was concentrated in vacuo and partitioned between dichloromethane and water. The organic layer was dried over anhydrous sodium sulfate and concentrated in vacuo to afford the desired compound as a pale yellow solid in quantitative yield.

According to the analysis of related databases, 689291-89-2, the application of this compound in the production field has become more and more popular.