Month: May 2021

These common heterocyclic compound, 25252-00-0, name is 2-Bromo-5-iodobenzoic acid, 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. Application In Synthesis of 2-Bromo-5-iodobenzoic acid

2-Bromo-5-iodobenzoic acid 5a (40.0 g, 122 mmol) was dissolved in dichloromethane (350 mL)Then, it was cooled to -5 C under a nitrogen atmosphere, and oxalyl chloride (16.4 mL, 194 mmol) was added dropwise.After reacting with N,N-dimethylformamide (1.5 mL, 19 mmol), the mixture was stirred at room temperature for 4 hours.After the reaction is completed, the organic solvent is removed by concentration under reduced pressure.The title compound 5b (46.0 g, yellow solid)Yield: 100%.

The synthetic route of 2-Bromo-5-iodobenzoic acid has been constantly updated, and we look forward to future research findings.

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, Recommanded Product: (5-Bromo-2-iodophenyl)methanol

A solution of oxalyl chloride (1.53 g, 0.012 mol) in CH2Cl2 (15 ML) was cooled to -70 C., and DMSO (1.41 g, 0.018 mol) in CH2Ck (15 ML) was added at -65 to -70 C. The mixture was stirred under nitrogen for 10 minutes at -70 C. and then treated with the product from Example 62B (2.35 g, 7.5 mmol) in 60 ML CH2Cl2.The slurry was stirred at -65 C. for 15 minutes and treated with triethylamine (3.8 g, 0.037 mol).The mixture was allowed to warm to -10 C. over 1 hour.The mixture was treated with 20 ML of water and allowed to warm to room temperature.The organic layer was separated and concentrated to provide the title compound. 1H NMR (CDCl3, 400 MHz) delta 9.97 (s, 1H), 7.97 (d, J=4 Hz, 1H), 7.79 (d, J=8 Hz, 1H), 7.40 (dd, J=4, 8 Hz, 1H). MS (DCl/NH3) [M+NH4]+ at 328.

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.

Reference of 328-73-4,Some common heterocyclic compound, 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene, molecular formula is C8H3F6I, 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: In a glovebox, aryl iodide (1.0 mmol), CsF (228 mg, 1.5 mmol), CuI (19.0 mg, 0.10 mmol), and PN-1 ligand (30 mg, 0.10 mmol) were weighed into a 4-dram borosilicate scintillation vial and dissolved in DMF (5 mL). Aryltriethoxysilane (1.0 mmol) was then added to the mixture, and the vial was tightly capped with a poly-seal conelined urea cap (Wheaton). The mixture was taken out of the glove box and placed in an oil bath pre-heated to 120 °C with vigorous stirring. After 48 h, the mixture was cooled to r.t., diluted with EtOAc (15 mL) and washed with H2O (3 × 5 mL). The aqueous fraction was back-extracted with EtOAc (3 × 5 mL). The combined organic fractions were dried (Na2SO4) and cotton-filtered, and the solvent was removed on a rotary evaporator. The product was purified by column chromatography (silica gel, hexanes, hexanes?Et2O, or hexanes?EtOAc).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Iodo-3,5-bis(trifluoromethyl)benzene, its application will become more common.

Related Products of 1320266-94-1,Some common heterocyclic compound, 1320266-94-1, name is 1-Iodo-3-isopropylimidazo[1,5-a]pyrazin-8-amine, molecular formula is C9H11IN4, 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.

N-(4-(8-amino-3-isopropylimidazo[l,5-a]pyrazin-l-yl)naphthalen-l-yl)-3- (trifluoromethyl)benzamide (GP146(Am)). A mixture of compound 1 (9.5 mg, 0.031 mmol), compound 4 (16.6 mg, 0.038 mmol), Tetrakis(triphenylphosphine)palladium (1.1 mg, 0.94 muetaiotaomicron) and sodium carbonate (7.3 mg, 0.069 mmol) was dissolved in a 3: 1 mixture of DME/water (120 muEpsilon). The mixture was heated overnight at 85 C. The crude mixture was cooled to room temperature, diluted in a mixture of acetonitrile/water and purified by reverse phase chromatography (HPLC) to obtain 5.3 mg of GP146(Am) (34% yield). TLC (CH2C12:MeOH, 95:5 v/v): Rf = 0.5; 1H NMR (300 MHz, MeOD) delta 8.46 (s, 1H), 8.42 (d, J = 6.0 Hz, 2H), 8.16- 8.13 (m, 1H), 8.01-7.98 (m, 1H), 7.86-7.84 (m, 1H), 7.81-7.77 (m, 2H), 7.72-7.69 (m, 1H), 7.68 – 7.62 (m, 2H), 7.60-7.54 (m, 1H), 7.06 (d, J = 6.0 Hz, 1H), 3.61 – 3.52 (m, 1H), 1.53 – 1.46 (m, 6H); ESI-MS (m/z): [M]+ calcd. for C27H22F3N50, 489.18; [M+l]+ found, 490.4 The purity of GP146(Am) was determined to be >98% by analytical HPLC.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Iodo-3-isopropylimidazo[1,5-a]pyrazin-8-amine, its application will become more common.

Electric Literature of 460-37-7, 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. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A solution of 880 mg (2.76 mmol) of the compound from Ex. 114A in 12 mL of DMF was treated with 1:35 g (4.15 mmol) cesium carbonate and stirred for 20 min at RT.Then 929 mg (4.15 mmol) 3,3,3-trifluoro-1-iodopropane were added, and the mixture was 2 h at 80 C heats.After cooling to RT was diluted with about 100 ml of ethyl acetate and washed twice with about 100 ml of water and once with 100 ml of saturated sodium chloride solution.After drying over anhydrous magnesium sulfate, was filtered and concentrated.The crude product was purified by preparative HPLC (method 6).The product fractions were combined and concentrated and the residue dried under high vacuum.There were 750 mg (63% d. Th.) Of the title compound.

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-3-iodopropane, other downstream synthetic routes, hurry up and to see.

Electric Literature of 25245-27-6, These common heterocyclic compound, 25245-27-6, name is 1-Iodo-3,5-dimethoxybenzene, 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.

EXAMPLE 20Synthesis of (1 S,2R,4a5,8a5)-1 -(3,5-dimethoxyphenoxymethyl)-2,5,5,8a-tetramethyl-decahydronaphthalen-2-ol (Compound No. 34) In a sealed tube purged with nitrogen, 1-iodo-3,5-dimethoxybenzene (Compound No. 31, 0.78 g, 2.95 mmol), (1S,2R,4a5,8a5)-1-(hydroxymethyl)-2,5,5,8a-tetramethyl-decahydronaphthalen-2-ol (Compound No. 26, 0.65 g, 2.68 mmol), Cs2CO3 (1.3 g, 3.99 mmol), 3,4,7,8-tetramethyl-[1,10]-phenylthroline (0.12 g, 0.50 mmol), Cul (0.05 g, 0.26 mmol), diglyme (2 mL) and toluene (10 mL) were added. The reaction mixture was stirred at 120C for 18 h. The reaction was cooled to room temperature, diluted with EtOAc (300 mL) and washed with water (100 mL). The organic layer was dried (Na2SO4) and concentrated. Purification by column chromatography on silica gel (Hexanes/EtOAc, 2:1) gave (1 S,2R,4aS,8aS)-1 -(3,5-dimethoxyphenoxymethyl)- 2,5,5,8a-tetramethyl-decahydronaphthalen-2-ol (Compound No. 34, 0.71 g, 70%) as a colorless oil. 1H NMR (CDCI3): 66.08 (s, 3H), 4.20 (m, 2H), 3.75 (s, 6H), 3.08 (s, 1H), 1.95-1.30 (m, 1OH), 1.30 (s, 3H), 1.25-1.00 (m, 2H), 0.90 (s, 6H), 0.88 (m, 2H), 0.80 (s, 3H).

The synthetic route of 25245-27-6 has been constantly updated, and we look forward to future research findings.

Some common heterocyclic compound, 52548-14-8, name is 2-Iodo-5-methylbenzoic acid, molecular formula is C8H7IO2, 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: 2-Iodo-5-methylbenzoic acid

Combine 1,2,3-triazole (3.45g, 50mmol), 2-iodo-5-methylbenzoic acid (5.24g, 20mmol), cesium carbonate (11.72g, 36mmol), trans-N, N ‘ -Dimethyl-1,2-cyclohexanediamine (0.51g, 3.6mmol), cuprous iodide (0.38g, 2mmol), N, N-dimethylformamide (30mL) were added to 100mL single-port round In a bottom flask, the temperature was gradually raised to 100 C under nitrogen protection for 4 hours. The reaction was stopped, cooled, diluted with tap water and extracted with ethyl acetate (200 mL × 2).The aqueous layer was acidified with concentrated hydrochloric acid (pH = 1-2) and extracted with ethyl acetate (200 mL × 2). The organic layers were combined, dried over anhydrous sodium sulfate, filtered, and the filtrate was evaporated to dryness under reduced pressure and purified by column chromatography ( Dichloromethane / methanol (v / v) = 50/1) gave the title compound (yellow solid, 2.76 g, 68%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 52548-14-8, its application will become more common.

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. 624-76-0, name is 2-Iodoethanol belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 2-Iodoethanol

Example 58Preparation of Derivative 58 According to the Present InventionDerivative 58 having the following formula was prepared as follows. Sodium hydride (24.14 mg, 1.0 mmol, 60% dispersed oil) was added in 20 ml of DMF solution containing 5-4-(2-cyclohexylethoxy)benzylidene)thiazolidin-2,4-dione (200 mg, 0.60 mmol) and stirred at room temperature under nitrogen. The mixture was further stirred for 10 minutes, and 2-iodoethanol (123.81 mg, 0.72 mmol) dissolved in 5 ml of DMF was slowly added thereto. After being stirred at 60 C. for 48 hours, the reaction mixture was extracted with ethyl acetate and washed with water. The organic layer was dried with anhydrous magnesium sulfate, filtered and solvent-evaporated. The residue was purified by silica gel chromatography (hexane:ethyl acetate=10:1) to afford Derivative 58 having the above formula, 5-[(4-(2-cyclohexylethoxy)benzylidene]-3-(hydroxyethyl)-1,3-thiazolidine-2,4-dione (180 mg, yield: 79%).1H NMR (300 MHz, CDCl3) delta 7.878 (s, 1H), 7.485 (d, J=14.4 Hz, 2H), 7.007 (d, J=14.4 Hz, 2H), 4.078 (t, J=13.2 Hz, 2H), 4.001 (t, J=10.2 Hz, 2H), 3.891 (t, J=10.2 Hz, 2H), 2.049 (m, 1H), 1.670-1.782 (m, 7H), 1.471-1.529 (m, 1H), 1.178-1.284 (m, 3H), 0.956-1.034 (m, 2H)

The synthetic route of 624-76-0 has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 1643-29-4, name is 3-(4-Iodophenyl)propanoic acid, 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. Safety of 3-(4-Iodophenyl)propanoic acid

Next, the 4-iodohydrocinnamic acid is methylated. 350 g of the produced 4-iodohydrocinnamic acid is wet with 250 g water. To the mixture is added 1.4 L methanol and 1.5 g p-toluene sulfonic acid in water. The mixture is refluxed overnight, and excess methanol is removed. 500 mL toluene is added and mixed, and then excess toluene and water is removed. Next, 500 mL methanol is added to the mixture. The mixture is refluxed for 30 minutes, after which excess methanol is again removed. The result is 162 g of methyl-4-iodohydrocinnamic acid (61% purity).

The synthetic route of 3-(4-Iodophenyl)propanoic acid has been constantly updated, and we look forward to future research findings.

Related Products of 156150-67-3,Some common heterocyclic compound, 156150-67-3, name is 2-Chloro-1-fluoro-4-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.

INTERMEDIATE 4; 2-(2-ChloiO-4-iodophenylamino)-5,5-dimethyl-8-oxo-5,6.7.8-tetrahydro-4H-thieno[“2,3- c”|azepine-3-carboxylic acid ethyl ester Caesium carbonate (2.77 g, 8.51 mmol) and 2-chloro-4-iodo-l-fluorobenzene(2.18 g, 8.51 mmol) were added to a solution of 2-amino-5,5-dimethyl-8-oxo-5, 6,7,8- tetrahydro-4i7-thieno[2,3-c]azepine-3-carboxylic acid ethyl ester (WO 2007/141504, Intermediate 20) (2.0 g, 7.09 mmol) in DMF (20 mL) and heated at 650C for 18 h. Brine (100 mL) was added to the reaction and the mixture extracted with DCM (3 x 50 mL). The combined organic extracts were dried (MgSO4) and concentrated in vacuo. The residual DMF was azeotroped with heptane. The crude product was purified by chromatography (silica, 0-30% EtOAc in DCM) to give the title compound as a cream solid (916 mg, 25%). deltaH (DMSO-d6) 10.60 (IH, s), 8.01 (IH, t, J 5.0 Hz), 7.95 (IH, d, J 2.0 Hz), 7.78 (IH, dd, J8.6, 2.0 Hz), 7.54 (IH, d, J8.6 Hz), 4.32 (2H, q, J7.1 Hz), 2.91 (2H, s), 2.85 (2H, d, J5.2 Hz), 1.33 (3H, t, J7.1 Hz), 0.99 (6H, s). LCMS (ES+) RT 3.81 minutes, 519 (M+H)+.

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