Month: May 2021

Some common heterocyclic compound, 76801-93-9, name is 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide, molecular formula is C14H18I3N3O6, 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: C14H18I3N3O6

In a three-necked flask equipped with a stirrer and a reflux condenser,5-amino-N, N’-bis- (2,3-dihydroxypropyl) -2,4,6-triiodo-1,3-benzenedicarboxamide (84.6 g, 0.12 mol)N, N-dimethylacetamide 172ml, stirred, heated to 50 C dissolved, cooled to 10 C, chloroacetyl chloride 62ml (88.09g, 0.78mol) dropwise over about 30min was completed, heated to 50 C and stirred for 3h, Cooled to 0 ~ 10 , at 10 ,156ml of 10mol / L sodium hydroxide solution was added dropwise and stirred at room temperature for 1h.100 ml of water was added and 59 ml of 1N hydrochloric acid was added dropwise. After standing overnight, the mixture was filtered and the filter cake was washed with water and dried to give 83.2 g. The yield was 90.0%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 76801-93-9, its application will become more common.

Related Products of 32337-97-6, 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. 32337-97-6 name is 1-Chloro-2-iodo-3-nitrobenzene, 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 stirred solution of l-chloro-2-iodo-3-nitrobenzene (143-2; 1.4 g, 0.00490 mol) in ethanol (20 mL) was added stannous chloride dihydrate (5.5 g, 0.0245 mol) portion wise at 0 C. Reaction mixture was allowed to stir at 70 C for 30 min. The reaction mixture was concentrated and diluted with ice cold water (150 mL) and PH was made slightly basic by addition of saturated aqueous sodium carbonate solution before being extracted with ethyl acetate (4 x 100 mL). The combined organic layer was washed with saturated aqueous sodium chloride solution, dried over sodium sulphate and concentrated under vacuum to obtain the title compound. 1H NMR (400 MHz, CDCI3) delta 7.048-7.008 (t, J = 8 Hz, 1 H), 6.713-6.693 (dd, J= 8, 8.8 Hz, 1 H), 6.655-6.632 (dd, J= 8.4, 9.2 Hz, 1 H), 5.5 (bs, 2 H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Chloro-2-iodo-3-nitrobenzene, and friends who are interested can also refer to it.

6136-66-9, name is (4-Iodophenyl)(phenyl)methanone, 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. Computed Properties of C13H9IO

Compound 23: 25-mL reaction flask was charged with 4-iodobenzophenone (0.5 mmol), 1-(p-toluenesulfonyl)indole-3-boronic acid (0.75 mmol), sodium carbonate (1.0 mmol), cesium hydroxide monohydrate. (2.5 mmol), sodium iodide (0.25 mmol), pivalic acid (0.75 mmol), chloroform (1.5 mmol) and ethylene glycol (2.0 g), reacted at 120 C for 24 h. Cool to room temperature, extract, the solvent was evaporated under reduced pressure and then purified by column chromatography to yield 84%.

The synthetic route of 6136-66-9 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 175278-30-5, A common heterocyclic compound, 175278-30-5, name is 4-Bromo-2-ethyl-1-iodobenzene, molecular formula is C8H8BrI, 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.

Compound (T-1) (10.0 g), 4-bromo-2-ethyl-1-iodobenzene (13.6 g), Tetrakis (triphenylphosphine) palladium(2.1 g), potassium carbonate (10.1 g), tetrabutylammonium bromide (1.18 g) and toluene (300 ml), IPA (80 ml) and pure water (20 ml) were charged into a reactor And the mixture was stirred at 90 ° C. for 5 hours. The reaction mixture was poured into water and the aqueous layer was extracted with toluene. The combined organic layers were washed with brine and dried over anhydrous magnesium sulfate. The solution was concentrated under reduced pressure, and the residue was purified by silica gel chromatography (volume ratio, heptane: toluene = 4: 1). (T-2) (12.6 g; 80percent) was obtained by further recrystallization from a mixed solvent of heptane and toluene (volume ratio, 4: 1).

The synthetic route of 175278-30-5 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 13421-13-1 as follows. Recommanded Product: 4-Chloro-2-iodobenzoic acid

General procedure: To a solution of imidazole carbaldehyde (1a-d) (100 mg, 1 equiv) in methanol (3 mL) were added successively Na2SO4 (0.2 g), amine 2a-d (1.2 equiv), alkynoic acid 3a-c (1.2 equiv) and isonitrile 4a-c (1.2 equiv) in a screw capped vial equipped with a magnetic stir bar. The reaction mixture was stirred at room temperature for 24-48 h in closed vial. After completion of the reaction, the mixture was diluted with dichloromethane (100 mL) and was extracted with water (50 mL). Organic layer was washed with brine (50 mL), dried over magnesium sulfate and evaporated under reduced pressure to obtained residue which was subjected to silica gel column chromatography (1-5 % methanol in dichloromethane) to afford the desired product 5a-r as solid.

According to the analysis of related databases, 13421-13-1, the application of this compound in the production field has become more and more popular.

Related Products of 31827-94-8, 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 31827-94-8 as follows.

General procedure: A sealed tube (35 mL) equipped with a stirring bar was loaded with 2-bromoethanones (1.0 mmol), then sodium benzenesulfinate (1.2 mmol) in DMF (20 mL) or phosphite (1.0 mmol) in toluene (20 mL) was added to the tube and the mixtures were stirred at room temperature till the 2-bromoethanones was totally consumed as indicated by TLC analysis (ca. 12 h for 1 and 24 h for 3). Then, the mixture was diluted with water (20 mL) and extracted with CH2Cl2 (30 mL x 3). Next, the organic phase was combined and dried over anhydrous Na2SO4. The solvent was removed by rotary evaporation and the oily mixture was purified with flash chromatograph column (elute: mixture of ethyl acetate and n-hexane), giving the desired products. And the 1H NMR spectra of the purified substrates were in accordance with the known literatures.

According to the analysis of related databases, 31827-94-8, the application of this compound in the production field has become more and more popular.

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. 628-77-3, name is 1,5-Diiodopentane, This compound has unique chemical properties. The synthetic route is as follows., Safety of 1,5-Diiodopentane

Example 19. (1 laS, 1 ia?S)-8,8-(pentane- 1 ,5-diylbis(oxy))bis(7-methoxy-2-methylene-23-dihydro- 1H-benzo[e]pyrrolo[ 1 ,2-aj [1 ,4jdiazepin-5( 11 aH)-one) (97) To a stirred suspended solution of Cs2CO3 (0.761 g, 2.33 mmol) in butanone (8 ml) were added (S)-8-hydroxy-7-methoxy-2-methyiene-2,3-dihydro- 1 H-benzo[e]pyrroio[ 1,2- aj[1,4jdiazepin-5(1 laH)-one (401 mg, 1.55 mmol) and 1,5-diiodopentane (240 mg, 0.740mmol). The mixture was stirred at RT overnight, concentrated, and purified on Si02 chromatography eluted with EtOAc/CH2C12 (1:10) to afford 337 rng (78% yield) of the title producL ElMS mlz 607.2 ([Mj+Na).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 628-77-3.

Related Products of 54413-93-3, 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. 54413-93-3, name is 2-Iodo-5-methoxybenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

1) Synthesis of 5-methoxy-2-(2H-1 ,2,3-triazol-2-yl)benzoic acid2-lodo-5-methoxy benzoic acid (15.0 g; 53.9 mmol) is dissolved in anhydrous DMF (45 ml) followed by the addition of 1 H-1 ,2,3-triazole (7.452 g; 108 mmol) and cesium carbonate (35.155 g; 108 mmol). By the addition of cesium carbonate the temperature of the reaction mixture increases to 40°C and gas evolved from the reaction mixture. Copper(l)iodide (514 mg; 2.7 mmol) is added. This triggers a strongly exothermic reaction and the temperature of the reaction mixture reaches 70°C within a few seconds. Stirring is continued for 30 minutes. Then the DMF is evaporated under reduced pressure followed by the addition of water (170 ml) and EtOAc (90 ml). The mixture is vigorously stirred and by the addition of citric acidmonohydrate the pH is adjusted to 3-4. The precipitate is filtered off and washed with water and EtOAc and discarded. The filtrate is poured into a separation funnel and the phases are separated. The water phase is extracted again with EtOAc. The combined organic layers are dried over MgS04, filtered and the solvent is evaporated to give 7.1 g of 5-methoxy-2-(2H- 1 ,2,3-triazol-2-yl)benzoic acid as a white powder of 94percent purity (6 percent impurity is the regioisomerically N1-linked triazolo-derivative); tR [min] = 0.60; [M+H]+ = 220.21

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-Iodo-5-methoxybenzoic acid, other downstream synthetic routes, hurry up and to see.

Electric Literature of 689260-53-5, The chemical industry reduces the impact on the environment during synthesis 689260-53-5, name is 2-Bromo-5-iodo-1,3-dimethylbenzene, I believe this compound will play a more active role in future production and life.

A mixture of 2-bromo-5-iodo-1 ,3-dimethylbenzene (500 mg), 1 ,2,4-triazole (340 mg), potassium carbonate (770 mg), and copper(l) iodide (232 mg) in N-methyl-2- pyrrolidinone is stirred at 130 C over night. More potassium carbonate (770 mg) and copper(l) iodide (232 mg) are added and the mixture is heated to 150 C for 4 h. After cooling to room temperature the mixture is diluted with tetrahydrofuran and filtered. The filtrate is concentrated in vacuo and purified by HPLC on reversed phase to give the title compound. LC (method 7): tR = 0.99 min; Mass spectrum (EST): m/z = 252, 254 [M+H]+.

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-Bromo-5-iodo-1,3-dimethylbenzene, 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. 13194-68-8, name is 4-Iodo-2-methylaniline, A new synthetic method of this compound is introduced below., category: iodides-buliding-blocks

(a) Preparation of 4Fluoro-2-(4iodo-2-methyl-phenylamino)-benzoic acid To a stirred solution containing 3.16 g (0.0133 mol) of 2-amino-5-iodotoluene in 5 mL of tetrahydrofuran at -78 C. was added 10 mL (0.020 mol) of a 2.0 M lithium diisopropylamide in tetrahydrofuran/heptane/ethylbenzene (Aldrich) solution. The resulting green suspension was stirred vigorously for 15 minutes, after which time a solution of 1.00 g (0.00632 mol) of 2,4-difluorobenzoic acid in 10 mL of tetrahydrofuran was added. The reaction temperature was allowed to increase slowly to room temperature, at which temperature the mixture was stirred for 2 days. The reaction mixture was concentrated by evaporation of the solvent under reduced pressure. Aqueous HCI (10%) was added to the concentrate, and the solution was extracted with dichloromethane. The organic phase was dried (MgSO4) and then concentrated over a steambath to low volume (10 mL) and cooled to room temperature. The off-white fibers which formed were collected by vacuum filtration, rinsed with hexane, and dried in a vacuum-oven (76 C.; ca. 10 mm of Hg) to afford 1.10 g (47%) of the desired material; mp 224-229.5 C.; 1H NMR (400 MHz, DMSO): delta 9.72 (s, 1H), 7.97 (dd, 1H, J=7.0, 8.7 Hz), 7.70 (d, 1H, J=1.5 Hz), 7.57 (dd, 1H,.J=8.4, 1.9 Hz), 7.17 (d, 1H, J=8.2 Hz), 6.61-6.53 (m, 2H), 2.18 (s, 3H); 13C NMR (100 MHz, DMSO): delta 169.87, 166.36 (d, JC-F=249.4 Hz), 150.11 (d, JC-F=11.4 Hz), 139.83, 138.49, 136.07, 135.26 (d, JC-F=11.5 Hz), 135.07, 125.60, 109.32, 104.98 (d, JC-F=21.1 Hz), 99.54 (d, JC-F=26.0 Hz), 89.43, 17.52; 19F NMR (376 MHz, DMSO): delta104.00 to -104.07 (m); IR (KBr) 1670 (C=O stretch)cm-1; MS (CI) M+1=372.

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.