82777-09-1 Archives - Iodides-buliding-blocks

Extended knowledge of 82777-09-1

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2′-Iodo-1,1′:3′,1”-terphenyl, and friends who are interested can also refer to it.

Electric Literature of 82777-09-1, 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. 82777-09-1 name is 2′-Iodo-1,1′:3′,1”-terphenyl, 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.

(2) Synthesis of Exemplified Compound A06 [0101] [Chem.[0102] The following reagents and solvents were charged into a 100-mL recovery flask. 21 -Iodo-m-terphenyl : 925 mg (2.60 mmol) TRP-Bpin2: 453 mg (0.943 mmol) Tetrakis (triphenylphosphine) palladium ( 0 ) : 80 mg (69 mu?iotaomicron) Toluene: 20 mLEthanol: 10 mL 30-wt% cesium carbonate aqueous solution: 10 mL This reaction solution was heat-refluxed for 3.5 hours while being stirred in a nitrogen atmosphere. After the reaction was completed, the reaction solution was added with water and was stirred, and a precipitated crystal was then filtrated, followed by performing washing with water, ethanol, and acetone, so that a crude product was obtained. Next, after this crude product was heated and dissolved in toluene, this solution thus obtained was filtrated while being hot, and recrystallization was then performed using toluene as a solvent. After the crystal thus obtained was vacuum dried at 150 C, sublimation refining was performed at a pressure of 10~4 Pa and a temperature of 360C, so that 251 mg of a high-purity exemplified compound A06 was obtained (yield: 39%) . [0103] The result of identification of the obtainedcompound is shown below. [MALDI-TOF-MS] Observed value: m/z=684.35, Calculated value:[1H-NMR (400 MHz, CDC13) ]delta 8.07 (d, 2H) , 8.04 (d, 2H) , 7.99 (dd, 2H) , 7.57-7.45 (m, 6H) , 7.41 (dd, 2H) , 7.18-7.00 (m, 22H) . In addition, the Tl energy (equivalent wavelength) of the exemplified compound A06 was 469 nm measured by a method similar to that of Example 1. [0104] When the energy gap of the exemplified compound A06 was further measured by a method similar to that of Example 1, the absorption edge of the absorption spectrum was 363 nm, and the energy gap of the exemplified compound A06 was 3.42 eV. [0105] When the ionization potential of the exemplified compound A06 was further measured by a method similar to that of Example 1, the ionization potential of theexemplified compound AO 6 was 6.34 eV. [0106] Furthermore, when the LUMO level of the exemplified compound A06 was estimated by a method similar to that of Example 1, it was estimated to be -2.92 eV.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2′-Iodo-1,1′:3′,1”-terphenyl, and friends who are interested can also refer to it.

Reference:
Patent; CANON KABUSHIKI KAISHA; KOSUGE, Tetsuya; KAMATANI, Jun; KISHINO, Kengo; TOMONO, Hiroyuki; WO2011/132624; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Simple exploration of 2′-Iodo-1,1′:3′,1”-terphenyl

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2′-Iodo-1,1′:3′,1”-terphenyl, its application will become more common.

Synthetic Route of 82777-09-1,Some common heterocyclic compound, 82777-09-1, name is 2′-Iodo-1,1′:3′,1”-terphenyl, molecular formula is C18H13I, 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 3 Synthesis of Exemplified Compound BOl[0107] [Chem. 14] [0108] The following reagents and solvents were charged into a 100-mL recovery flask. 2 , 8-Dibromodibenzothiophene : 600 mg (1.75 mmol) ( 1 , 3-Bis (diphenylphosphino) propane ) dichloronickel ( II ) : 380 mg (0.70 mmol)Toluene: 24 mLTriethylamine : 1.46 mL After this reaction solution was heated to 90C and was then added with 1.53 mL (10.5 mmol) of 4 , 4 , 5, 5-tetramethyl- 1, 3, 2-dioxaborolane, heating was performed for 6.5 hours. After the reaction solution was cooled to room temperature, the reaction was quenched by addition of water, and an insoluble matter was removed by filtration of the reaction solution. After a reaction product in the filtrate was extracted using toluene, this extracted solution was washed with water and was then dried over sodium sulfate, followed by concentration, so that a crude product was obtained. The obtained crude product was refined by a silica gel column chromatography (eluent: toluene), and 124 mg of intermediate S-Bpin2 was obtained (yield: 16%) . [0109] Then, the following reagents and solvents were charged into a 50-mL recovery flask. 2 ‘ -Iodo-m-terphenyl: 245 mg (0.688 mmol) S-Bpin2:120 mg (0.275 mmol) Tetrakis ( triphenylphosphine ) palladium ( 0 ) : 25 mg (22 umol) Toluene: 6 mLEthanol: 3 mL 30-wt% cesium carbonate aqueous solution: 3 mL This reaction solution was heat-refluxed for 4.5 hours while being stirred in a nitrogen atmosphere. After the reaction was completed, the reaction solution was washed with water and was then dried over sodium sulfate, followed by concentration, so that a crude product was obtained.Next, this crude product was refined by a silica gel column chromatography (eluent: heptane/chloroform=3/l ) , and heating dispersion washing was further performed using a mixed solvent containing hexane and ethanol. After a crystal thus obtained was vacuum dried at 150C, sublimation refining was performed at a pressure of 10~4 Pa and a temperature of 340C, so that 120 mg of a high-purity exemplified compound B01 was obtained (yield: 68%). [0110] The result of identification of the obtainedcompound is shown below. [MALDI-TOF-MS] Observed value:[1H-N R (400 MHz, CDC13) ]delta 7.75-7.42 (m, 6H) , 7.35 (d, 2H) , 7.16-7.01 (m, 22H) , 6.85 (dd, 2H) . In addition, the Tl energy (equivalent wavelength) of the exemplified compound B01 was 423 nm measured by a method similar to that of Example 1. [0111] When the energy gap of the exemplified compound B01 was further measured by a method similar to that of Example 1, the absorption edge of the absorption spectrum was 322 nm, and the energy gap of the exemplified compound B01 was 3.85 eV. [0112] In addition, when the ionization potential of the exemplified compound B01 was measured by a method similar to that of Example 1, 6.49 eV was obtained. [0113] Furthermore, when the LUMO level of the exemplified compound B01 was estimated by a method similar to that of Example 1, it was estimated to be -2.64 eV.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2′-Iodo-1,1′:3’,1”-terphenyl, its application will become more common.

New learning discoveries about 82777-09-1

The synthetic route of 82777-09-1 has been constantly updated, and we look forward to future research findings.

82777-09-1, name is 2′-Iodo-1,1′:3′,1”-terphenyl, 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 C18H13I

(2) In a 50-mL reaction container, XX-2 (109 mg, 0.243 mmol) and XX-3 (190.4 mg, 0.535 mmol) were mixed in a toluene/ethyl alcohol (3 mL/1.5 mL) mixture solvent, and dissolved oxygen was removed by nitrogen. Note that XX-3 is a compound synthesized in accordance with the procedure described in The Journal of Organic Chemistry, 51, 3162 (1986). Then, Pd(PPh3)4 (14.0 mg, 0.01215 mmol) and an aqueous solution of 2 M cesium carbonate (1.5 mL) were added to the mixture under a nitrogen atmosphere, followed by heating to 85C and reaction at the temperature for 12 hours. The reaction solution was cooled to room temperature,concentrated under reduced pressure, and subjected to silica gel chromatography (mobile phase: hexane/toluene = 3/1) for isolation and purification to obtain A-2 (35 mg, yield: 17%) as a white solid powder.[0083] Mass-spectrometry (MS) and nuclear magneticresonance spectrometry (NMR) of compound A-2 gave theresults that the molecular weight and the ratio ofintegrated values of NMR peaks well agreed with thestructure of compound A-2. Specifically, 846 as M+ of this compound was confirmed by matrix-assisted laser desorption- ionization mass spectrometry (MALDI-MS) . The measurement results of nuclear magnetic resonance spectrometry are shown below :1H-NMR (THF-d8) ? (ppm) : 7.52 (t, 2H) , 7.42 (d, 4H) , 7.38 (d, 2H) , 7.25 (m, 8H) , 7.19-7.11 (m, 12H) , 6.70 (s, 2H) .13C-NMR (THF-ds) ? (ppm): 142.31, 140.43, 139.64, 139.51, 139. 24, 130.03, 129.25, 128.29, 127.93, 127.16, 126.39, 125.24, 124.45, 121.91, 119.25.

The synthetic route of 82777-09-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CANON KABUSHIKI KAISHA; YAMADA, Kenji; OKADA, Shinjiro; WO2012/2185; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some tips on 82777-09-1

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 82777-09-1, its application will become more common.

Some common heterocyclic compound, 82777-09-1, name is 2′-Iodo-1,1′:3′,1”-terphenyl, molecular formula is C18H13I, 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. category: iodides-buliding-blocks

General procedure: The outline of our synthetic routes to the 6 compounds listed in Fig. 1 is shown in Scheme 1. They were synthesized by Suzuki-Miyaura coupling of 2,6-dibromodithieno[3,2-b:2?,3?-d]thiophene each with the corresponding boronic acid. Compounds 5 and 7 in Fig. 1 were also synthesized by Suzuki-Miyaura coupling of 3,7-bis(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)dibenzo[b,d]thiophene and 2,6-bis(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)dithieno[3,2-b:2?,3?-d]thiophene with 2?-iodo-1,1?:3?,1?-terphenyl, respectively. The typical procedure is following. A mixture of 2,6-dibromo-dithieno[3,2-b:2?,3?-d]thiophene (174.0 mg, 0.5 mmol), boronic acid of counterpart (1.5 mmol), tetrakis (triphenylphosphine) palladium (81.5 mg, 0.08 mmol) and Cs2CO3 (2.0 mL, 2.0 M in aqueous) in 8 mL solvent of toluene: THF = 1:1 was stirred at reflux temperature for 8 h. All reactions were carried out under nitrogen atmosphere with anhydrous solvents. The mixture was poured into water (30 mL) and extracted with CH2Cl2 (20 mL ¡Á 3). The combined extract was washed with brine (40 mL), dried (Na2SO4), and concentrated in vacuo. Column chromatography on silica gel eluted with CHCl3:toluene = 1:1. All compounds were characterized by 1H and 13C NMR and mass spectroscopy.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 82777-09-1, its application will become more common.

Reference:
Article; Okada, Shinjiro; Yamada, Kenji; Journal of Molecular Structure; vol. 1037; (2013); p. 256 – 263;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Introduction of a new synthetic route about 82777-09-1

Related Products of 82777-09-1,Some common heterocyclic compound, 82777-09-1, name is 2′-Iodo-1,1′:3′,1”-terphenyl, molecular formula is C18H13I, 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.